CN106111156A - Efficient class Fenton magnetic catalyst based on clay mineral and preparation method and application - Google Patents
Efficient class Fenton magnetic catalyst based on clay mineral and preparation method and application Download PDFInfo
- Publication number
- CN106111156A CN106111156A CN201610470204.0A CN201610470204A CN106111156A CN 106111156 A CN106111156 A CN 106111156A CN 201610470204 A CN201610470204 A CN 201610470204A CN 106111156 A CN106111156 A CN 106111156A
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- Prior art keywords
- 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 17
- 239000000243 solution Substances 0.000 claims abstract description 23
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 20
- 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 13
- 229910052751 metal Inorganic materials 0.000 claims abstract description 13
- 239000000725 suspension Substances 0.000 claims abstract description 12
- 230000008569 process Effects 0.000 claims abstract description 11
- 239000002184 metal Substances 0.000 claims abstract description 8
- 239000002957 persistent organic pollutant Substances 0.000 claims abstract description 8
- 238000001556 precipitation Methods 0.000 claims abstract description 7
- 239000012266 salt solution Substances 0.000 claims abstract description 7
- 239000007787 solid Substances 0.000 claims abstract description 6
- 239000003513 alkali Substances 0.000 claims abstract description 3
- 150000003839 salts Chemical class 0.000 claims abstract description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 28
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 24
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 18
- 239000002689 soil Substances 0.000 claims description 10
- 238000006243 chemical reaction Methods 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
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 230000003197 catalytic effect Effects 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
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- 229910052802 copper Inorganic materials 0.000 claims description 6
- 239000010949 copper Substances 0.000 claims description 6
- 229910052742 iron Inorganic materials 0.000 claims description 6
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 5
- 229910052721 tungsten Inorganic materials 0.000 claims description 5
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 5
- 239000010937 tungsten Substances 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
- 150000001875 compounds Chemical class 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 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
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 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
- 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
- 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
- 231100000614 poison Toxicity 0.000 claims description 2
- 230000007096 poisonous effect Effects 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims 1
- 229910000859 α-Fe Inorganic materials 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 15
- 238000006555 catalytic reaction Methods 0.000 abstract description 11
- 230000015556 catabolic process Effects 0.000 abstract description 6
- 238000006731 degradation reaction Methods 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 5
- 230000007935 neutral effect Effects 0.000 abstract description 4
- 231100000331 toxic Toxicity 0.000 abstract description 4
- 230000002588 toxic effect Effects 0.000 abstract description 4
- 235000013980 iron oxide Nutrition 0.000 description 19
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 14
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical class [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 239000000463 material Substances 0.000 description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 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
- 229960002089 ferrous chloride Drugs 0.000 description 6
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 6
- 238000003756 stirring Methods 0.000 description 5
- 239000002351 wastewater Substances 0.000 description 5
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 4
- 239000011812 mixed powder Substances 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000008859 change Effects 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
- 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
- -1 iron oxides compound Chemical class 0.000 description 2
- 229910000358 iron sulfate Inorganic materials 0.000 description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 235000010755 mineral Nutrition 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
- 230000001476 alcoholic effect Effects 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 229960000892 attapulgite Drugs 0.000 description 1
- 239000000987 azo dye Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect 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
- 230000007547 defect 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
- 238000002474 experimental method Methods 0.000 description 1
- PGBHMTALBVVCIT-VCIWKGPPSA-N framycetin Chemical compound N[C@@H]1[C@@H](O)[C@H](O)[C@H](CN)O[C@@H]1O[C@H]1[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](N)C[C@@H](N)[C@@H]2O)O[C@@H]2[C@@H]([C@@H](O)[C@H](O)[C@@H](CN)O2)N)O[C@@H]1CO PGBHMTALBVVCIT-VCIWKGPPSA-N 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
- 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
- 230000007774 longterm Effects 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
- 239000002905 metal composite material Substances 0.000 description 1
- 238000002156 mixing Methods 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
- 230000002688 persistence Effects 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
- 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
Landscapes
- 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 present invention relates to a kind of efficient class Fenton magnetic catalyst based on clay mineral and preparation method and application.Preparation process is: clean clay mineral is added in the iron salt solutions prepared in advance by (1), makes mixed suspension be warmed up to 60 100 DEG C and continuously stirred 0.5 5 hours reach stable；(2) adding alkali liquor in suspension makes solution ph rise to 8 11, and continuously stirred 0.5 6 hours, the processes such as solid precipitation is scrubbed, dry obtained Precursor Powder；(3) during Precursor Powder impregnated in the solution containing other nonferrous metal salt, uniformly it is evaporated, heat treatment, i.e. obtains efficient class Fenton magnetic catalyst based on clay mineral.Compared with prior art, the catalyst of the present invention has Magneto separate, it is possible to reclaims and recycles, and has efficient class Fenton catalysis activity and stability under near neutral pH simultaneously.The preparation technology of this catalyst is simple, and cost is relatively low and ecological compatibility good, has broad prospect of application in difficult degradation toxic organic pollutant process field.
Description
Technical field
The invention belongs to inorganic nanometer functional material and environmental pollution control technique field, especially relate to a kind of based on viscous
The soil efficient class Fenton magnetic catalyst of mineral and preparation method and application.
Background technology
The situation is tense in the pollution of surface water, subsoil water and soil that China is current, wherein with pesticide, Antibiotique composition,
The difficult degradation persistence organic pollutant such as polycyclic aromatic hydrocarbon, azo dye is the polluter of representative, at the ring that we depend on for existence
, irreversible potential threat will be there is to the health of ecological environment and people in the medium-term and long-term existence in border.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 such as change, occupy critical role in terms of persistency toxic organic pollutant in removing environment.Wherein, heterogeneous class Fenton
Chemical oxidization method, by utilizing heterogeneous catalysis material catalytic activation hydrogen peroxide or persulfate etc. to produce the hydroxyl of Strong oxdiative certainly
By base, thus the toxic organic pollutant thoroughly decomposing and eliminating in environment, it is a kind of more practical persistency organic contaminant
Control technology.Such as, the Chinese patent of Publication No. CN103230796A discloses a kind of attapulgite load ferroso-ferric oxide
Preparation method, this Magneto separate material may be used for class Fenton's reaction degradable organic pollutant, and reclaimed by Magneto separate and urge
Formed material.But the catalysis activity of the catalyst based on ferroso-ferric oxide is more weak.The most also there is other burning of employing
Thing discloses a kind of nanometer as the Chinese patent of the report of carrier loaded iron oxides, such as Publication No. CN105536812A
Fe3O4/Mn3O4Composite, and there is Magneto separate and the feature of class Fenton catalytic degradation organic pollution.But these are with ferrum
Oxide is main catalyst, and its effective range is narrower, generally can play significantly catalysis in the pH scope less than 4
Degradation effect, and once pH value of solution is more than 4, is little to produce any catalytic action.Because asking in view of the corrosion-resistant of reactor
Topic, ferrum dissolution problem under acid condition and add the problems such as increase technical costs that soda acid causes, 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 of break-through skill bottleneck.
The Chinese patent of Publication No. CN105405567A discloses the magnetic of a kind of layered clay mineral supported ferriferous oxide
Property material for the soil of Organic Pollution or the reparation of water, the method can be controlled the composition of magnetic iron oxide by roasting
With structure keep the magnetic characteristic that material is good, and the method proposes to add mixing of non-ferric while preparing iron oxides
Miscellaneous metallic element so that magnetic material also has obvious catalytic effect pH value is close to 4 when.But this method can be drawn
The doping metals entered is the lowest, only the 0.1-5% of ferrum, because the content of higher-doped metal will cause doping metals and ferrum oxygen
The interaction of compound forms nonmagnetic metal composite oxide, causes the disappearance of final catalysis material magnetic.The most how
It is very important skill that raising nonferrous metal content, enhancing near neutral pH are catalyzed active, simultaneously to keep catalysis material magnetic
Art problem.
Summary of the invention
Defect that the purpose of the present invention is contemplated to overcome above-mentioned prior art to exist and provide a kind of based on clay mineral
Efficient class Fenton magnetic catalyst and preparation method and application.
Present invention thought based on " take from soil, be used for soil ", uses the layered clay mineral that environment compatibility is good
Based on material, introduce thereon and there is the iron oxides of superparamagnetic performance, reclaim and recycle reaching quick Magneto separate
Purpose；Meanwhile, the present invention passes through after iron oxides is stablized in formation, before heat treatment, introduces higher containing by infusion process
The preferred nonferrous metal salt of amount, is allowed to deposit and in heat treatment process at the clay mineral of substrate and the surface of iron oxides
Being decomposed to form metal-oxide, maintain the crystal phase structure of magnetic iron oxide, final acquisition catalysis activity is high, having can
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
Other metal-oxide, wherein magnetic iron oxide is 0.05-2 with the mass ratio of clay mineral, other metal-oxide and magnetic
The mol ratio of property iron oxides is 0.1-1, and other described metal-oxide is in manganese metal, cobalt, aluminum, copper, zirconium or tungsten
Plant or two oxides.
Described clay mineral has layer structure, in bentonite, illite or montmorillonite one or both
Combination.
The preparation method of described based on clay mineral efficient class Fenton magnetic catalyst, comprises the following steps:
(1) clean clay mineral is added in the iron salt solutions prepared in advance, makes mixed suspension be warmed up to
Reach stable for 60-100 DEG C and continuously stirred 0.5-5 hour；
(2) adding alkali liquor in suspension makes solution ph rise to 8-11, continuously stirred 0.5-6 hour, solid precipitation
The process such as scrubbed, dry obtains Precursor Powder；
(3) during Precursor Powder impregnated in the solution containing other slaine, uniformly it is evaporated, heat treatment, i.e. obtains based on clay
The efficient class Fenton magnetic catalyst of mineral.
Described iron salt is the mixture of any solubility divalent iron salt or bivalence and trivalent iron salt, wherein preferred ferrous iron
Being 0.3-3 with ferric iron mol ratio, total concentration of iron is 0.1-5 mol/L.
Other slaine described is one or both the water solublity in metallic element manganese, cobalt, aluminum, copper, zirconium or tungsten or alcohol
Soluble, the most preferably nitrate, sulfate, hydrochlorate or the complex containing ammonium root, the molar concentration of other slaine is
0.05-2 mol/L, other metallic element is 0.1-1 with the mol ratio of ferrum.
Described being evaporated operates into the heating evaporation less than 100 DEG C.
The heating rate of described heat treatment is 1-20 DEG C/min, and the temperature of heat treatment is 200-600 DEG C, the time of heat treatment
For 1-48 hour, the atmosphere of heat treatment was air.
Described based on clay mineral efficient class Fenton magnetic catalyst can be used for efficient catalytic and decomposes hydrogen peroxide generation
Poisonous persistent organic pollutants in water or soil are decomposed and are removed, can be reclaimed by Magneto separate simultaneously by class Fenton's reaction
Utilize.
Compared with prior art, the present invention has the following advantages and beneficial effect:
(1) containing magnetic iron oxide in the catalyst of the present invention, therefore, catalyst has Magneto separate, it is possible to return
Receive and recycle.
(2) in the catalyst of the present invention, possibly together with the oxide of manganese metal, cobalt, aluminum, copper, zirconium or the tungsten of other non-ferric, this
The metal-oxide of a little non-ferric, with under iron oxides compound action, can have under the conditions of near neutral pH and urge efficiently
Change and decompose hydrogen peroxide generation high activity hydroxyl radical free radical, play the effect of class Fenton's reaction, this is because these metal-oxides
Surface isoelectric point, IP is caused to decline after compound with iron oxides, namely near neutral pH lower surface with higher nagative potential,
Catalyst surface forms the region of rich proton so that absorbability and catalytic decomposition ability to hydrogen peroxide improve, thus play
Purifying organic polluted water or the function of soil.
The present invention strictly controls the proportioning of clay mineral, iron oxides and nonferrous metal oxides, and by a large amount of
Experimental verification clay mineral, the content of iron oxides, the selection of nonferrous metal element and addition etc. are for catalyst performance
Impact, finally draws the magnetic heterogeneous class fenton catalyst of the present invention.
Synthesis technique of the present invention is simple, and equipment requirements is low, with low cost, and catalyst eco-compatibility is good；Use catalyst
Carry out heterogeneous class Fenton's reaction and can efficiently remove the organic pollution in environment in wide pH scope, react non-secondary pollution,
Economically feasible, the difficult degradation toxic organic pollutant process field at waste water and soil has broad application prospects.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in detail.
The catalysis activity experiment measuring by degradation of phenol.Phenol concentration employing chromatograph of liquid (HPLC-2010A,
Shimadzu) measure, total organic carbon employing total organic carbon analyzer (TOC-V-TN analyzer, multi N/C 3000,
Analytic Jena, Germany) measure.
Embodiment 1
(1) clean Kaolin is added in ferrous sulfate and ferrum sulfuricum oxydatum solutum, by iron oxides and kaolinic reason
Opinion mass ratio is 0.05, ferrous sulfate and iron sulfate mol ratio are 0.3, total iron content is that 0.1 mol/L carries out iron salt solutions
Preparation.Suspension is warmed up to 60 DEG C and continuously stirred 0.5 hour reach stable；
(2) adding the sodium hydroxide of 5 mol/L in suspension makes solution ph rise to 8, continuously stirred 0.5 hour；
The processes such as solid precipitation is scrubbed, dry obtain Precursor Powder；
(3), during Precursor Powder impregnated in the manganese nitrate aqueous solution of 0.05 mol/L, wherein manganese is 0.1 with the mol ratio of ferrum,
Agitating solution is also evaporated, and dried mixed-powder is placed in air atmosphere, is warmed up in 200 DEG C of air at heat with 1 DEG C/min
Manage 1 hour, efficient class Fenton magnetic catalyst can be obtained.
(4) above-mentioned catalyst treatment is contained the wastewater test performance of phenol.It is 100 mg/litre, initial pH at initial concentration
It is that the phenol solution of 4.5 adds the catalyst of 0.1 grams per liter and the hydrogen peroxide of 30 mM/ls, after stirring reaction 30 minutes,
Phenol concentration declines 80%, and total organic carbon declines 50%.Use Magneto separate reclaim catalyst and recycle three times, be finally catalyzed
Activity is more than the 90% of first use activity.
Embodiment 2
(1) clean bentonite is added in ferrous chloride and ferric chloride solution, by iron oxides and kaolinic reason
Opinion mass ratio is 2, ferrous chloride and iron chloride mol ratio are 3, total iron content is the preparation that 5 mol/L carry out iron salt solutions.Outstanding
Turbid liquid is warmed up to 100 DEG C and continuously stirred 5 hours reach stable；
(2) adding the sodium hydroxide of 2 mol/L in suspension makes solution ph rise to 11, continuously stirred 6 hours；
The processes such as solid precipitation is scrubbed, dry obtain Precursor Powder；
(3) during Precursor Powder impregnated in the copper nitrate aqueous solution of 2 mol/L, wherein copper is 1 with the mol ratio of ferrum, stirring
Solution is also evaporated, and dried mixed-powder is placed in air atmosphere, is warmed up to heat treatment 48 in 600 DEG C of air with 20 DEG C/min
Hour, efficient class Fenton magnetic catalyst can be obtained.
(4) catalyst treatment test performance of waste water containing phenol: initial concentration be 50 mg/litre, initial pH be 5
Phenol solution adds the catalyst of 1 grams per liter and the hydrogen peroxide of 50 mM/ls, after stirring reaction 60 minutes, under phenol concentration
Fall 92%, total organic carbon declines 60%.Using Magneto separate reclaim catalyst and recycle three times, final catalysis activity is first
Use more than the 95% of activity.
Embodiment 3
(1) clean illite is added in ferrous chloride and ferrum sulfuricum oxydatum solutum, by iron oxides and kaolinic reason
Opinion mass ratio is 1, ferrous chloride and iron sulfate mol ratio are 2, total iron content is the preparation that 1 mol/L carries out iron salt solutions.Outstanding
Turbid liquid is warmed up to 80 DEG C and continuously stirred 2 hours reach stable；
(2) adding the sodium hydroxide of 1 mol/L in suspension makes solution ph rise to 9, continuously stirred 2 hours；Gu
The processes such as body precipitation is scrubbed, dry obtain Precursor Powder；
(3) during Precursor Powder impregnated in copper nitrate and the aluminum nitrate aqueous solution of 1 mol/L, Qi Zhongtong: aluminum: ferrum mole
Ratio is 1:1:5, and agitating solution is also evaporated, and dried mixed-powder is placed in air atmosphere, is warmed up to 450 DEG C with 10 DEG C/min
Heat treatment 24 hours in air, can obtain efficient class Fenton magnetic catalyst.
(4) catalyst treatment test performance of waste water containing phenol: initial concentration be 60 mg/litre, initial pH be 4.8
Phenol solution in add the catalyst of 0.5 grams per liter and the hydrogen peroxide of 40 mM/ls, after stirring reaction 30 minutes, phenol is dense
Degree decline 96%, total organic carbon declines 70%.Using Magneto separate reclaim catalyst and recycle three times, final catalysis activity is
More than the 96% of first use activity.
Embodiment 4
(1) clean bentonite is added in ferrous chloride and ferric chloride solution, by iron oxides and kaolinic reason
Opinion mass ratio is 0.5, ferrous chloride and iron chloride mol ratio are 1, total iron content is that 0.5 mol/L carries out joining of iron salt solutions
System.Suspension is warmed up to 90 DEG C and continuously stirred 3 hours reach stable；
(2) adding the sodium hydroxide of 3 mol/L in suspension makes solution ph rise to 10, continuously stirred 2 hours；
The processes such as solid precipitation is scrubbed, dry obtain Precursor Powder；
(3) during Precursor Powder impregnated in the alcoholic solution of nitrification cobalt hexamine complex of 2 mol/L, wherein cobalt and ferrum
Mol ratio is 0.5, and agitating solution is also evaporated, and dried mixed-powder is placed in air atmosphere, is warmed up to 500 with 5 DEG C/min
In DEG C air, heat treatment 12 hours, can obtain efficient class Fenton magnetic catalyst.
(4) catalyst treatment test performance of waste water containing phenol: initial concentration be 100 mg/litre, initial pH be 6
Phenol solution in add the catalyst of 0.5 grams per liter and the hydrogen peroxide of 30 mM/ls, after stirring reaction 20 minutes, phenol is dense
Degree decline 99%, total organic carbon declines 70%.Using Magneto separate reclaim catalyst and recycle three times, final catalysis activity is
More than the 98% of first use activity.
The above-mentioned description to embodiment is to be understood that for ease of those skilled in the art and use invention.
These embodiments obviously easily can be made various amendment by person skilled in the art, and described herein typically
Principle is applied in other embodiments without through performing creative labour.Therefore, the invention is not restricted to above-described embodiment, ability
Field technique personnel should be the present invention's according to the announcement of the present invention, the improvement made without departing from scope and amendment
Within protection domain.
Claims (8)
1. an efficient class Fenton magnetic catalyst based on clay mineral, it is characterised in that include clay mineral, magnetic ferrite
Compound and other metal-oxide, wherein magnetic iron oxide is 0.05-2 with the mass ratio of clay mineral, other metal oxygen
The mol ratio of compound and magnetic iron oxide is 0.1-1, other described metal-oxide be manganese metal, cobalt, aluminum, copper, zirconium or
One or both oxides in tungsten.
A kind of efficient class Fenton magnetic catalyst based on clay mineral the most according to claim 1, it is characterised in that institute
The clay mineral stated has layer structure, one or both the combination in bentonite, illite or montmorillonite.
3. a preparation method for efficient class Fenton magnetic catalyst based on clay mineral as claimed in claim 1, it is special
Levy and be, comprise the following steps:
(1) clean clay mineral is added in the iron salt solutions prepared in advance, makes mixed suspension be warmed up to 60-
Reach stable for 100 DEG C and continuously stirred 0.5-5 hour；
(2) adding alkali liquor in suspension makes solution ph rise to 8-11, and continuously stirred 0.5-6 hour, solid precipitation was through washing
The process such as wash, be dried obtains Precursor Powder；
(3) during Precursor Powder impregnated in the solution containing other slaine, uniformly it is evaporated, heat treatment, i.e. obtains based on clay mineral
Efficient class Fenton magnetic catalyst.
The preparation method of efficient class Fenton magnetic catalyst based on clay mineral the most according to claim 3, its feature
Being, described iron salt is the mixture of any solubility divalent iron salt or bivalence and trivalent iron salt, wherein preferably ferrous iron with
Ferric iron mol ratio is 0.3-3, and total concentration of iron is 0.1-5 mol/L.
The preparation method of efficient class Fenton magnetic catalyst based on clay mineral the most according to claim 3, its feature
Being, other slaine described is one or both the water solublity in metallic element manganese, cobalt, aluminum, copper, zirconium or tungsten or alcohol-soluble
Salt, the most preferably nitrate, sulfate, hydrochlorate or the complex containing ammonium root, the molar concentration of other slaine is 0.05-
2 mol/L, other metallic element is 0.1-1 with the mol ratio of ferrum.
The preparation method of efficient class Fenton magnetic catalyst based on clay mineral the most according to claim 3, its feature
Be, described in be evaporated into less than 100 DEG C heating evaporation operate.
The preparation method of efficient class Fenton magnetic catalyst based on clay mineral the most according to claim 3, its feature
Being, the heating rate of described 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
1-48 hour, the atmosphere of heat treatment was air.
8. an application for efficient class Fenton magnetic catalyst based on clay mineral as claimed in claim 1, its feature exists
In, described based on clay mineral efficient class Fenton magnetic catalyst can be used for efficient catalytic and decomposes hydrogen peroxide generation class Fenton
Poisonous persistent organic pollutants in water or soil are decomposed and are removed, can be recycled by Magneto separate simultaneously by reaction.
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