CN106076339A - A kind of preparation method of magnetic synergistic oxidation Co catalysts - Google Patents
A kind of preparation method of magnetic synergistic oxidation Co catalysts Download PDFInfo
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- CN106076339A CN106076339A CN201610407770.7A CN201610407770A CN106076339A CN 106076339 A CN106076339 A CN 106076339A CN 201610407770 A CN201610407770 A CN 201610407770A CN 106076339 A CN106076339 A CN 106076339A
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- 239000003426 co-catalyst Substances 0.000 title claims abstract description 17
- 230000003647 oxidation Effects 0.000 title claims abstract description 16
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 16
- 230000002195 synergetic effect Effects 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 claims abstract description 24
- 229960001545 hydrotalcite Drugs 0.000 claims abstract description 23
- 229910001701 hydrotalcite Inorganic materials 0.000 claims abstract description 23
- 150000001875 compounds Chemical class 0.000 claims abstract description 21
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 19
- 239000010941 cobalt Substances 0.000 claims abstract description 19
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 18
- 239000007789 gas Substances 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 9
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910021577 Iron(II) chloride Inorganic materials 0.000 claims abstract description 6
- CKUAXEQHGKSLHN-UHFFFAOYSA-N [C].[N] Chemical compound [C].[N] CKUAXEQHGKSLHN-UHFFFAOYSA-N 0.000 claims abstract description 6
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims abstract description 6
- 229940097267 cobaltous chloride Drugs 0.000 claims abstract description 6
- 230000001351 cycling effect Effects 0.000 claims abstract description 6
- JHJUUEHSAZXEEO-UHFFFAOYSA-M sodium;4-dodecylbenzenesulfonate Chemical compound [Na+].CCCCCCCCCCCCC1=CC=C(S([O-])(=O)=O)C=C1 JHJUUEHSAZXEEO-UHFFFAOYSA-M 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 239000002244 precipitate Substances 0.000 claims description 10
- 238000001556 precipitation Methods 0.000 claims description 10
- 230000000694 effects Effects 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- 238000002242 deionisation method Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- 239000004575 stone Substances 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- 239000003344 environmental pollutant Substances 0.000 abstract description 2
- 231100000719 pollutant Toxicity 0.000 abstract description 2
- 239000013049 sediment Substances 0.000 abstract 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 18
- 239000003054 catalyst Substances 0.000 description 11
- 239000000463 material Substances 0.000 description 8
- 230000015556 catabolic process Effects 0.000 description 7
- 238000006731 degradation reaction Methods 0.000 description 7
- 239000011229 interlayer Substances 0.000 description 5
- 150000001450 anions Chemical class 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 229910052599 brucite Inorganic materials 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 150000001768 cations Chemical class 0.000 description 3
- 229910000428 cobalt oxide Inorganic materials 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 2
- -1 compound anion Chemical class 0.000 description 2
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 1
- 240000002853 Nelumbo nucifera Species 0.000 description 1
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001449 anionic compounds Chemical class 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 150000001869 cobalt compounds Chemical class 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003933 environmental pollution control Methods 0.000 description 1
- 229910001448 ferrous ion Inorganic materials 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000007943 implant Substances 0.000 description 1
- 229910001412 inorganic anion Inorganic materials 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 150000002891 organic anions Chemical class 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 239000002699 waste material Substances 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
- B01J23/70—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
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention discloses the preparation method of a kind of magnetic synergistic oxidation Co catalysts.In turn include the following steps: under the conditions of water bath with thermostatic control, FeCl2Solution drips hydrogen peroxide and NaOH weak solution, proceeds to after stirring in autoclave, continue reaction, naturally cool to room temperature, obtain solid sediment, add it to, in dodecylbenzene sodium sulfonate solution, obtain magnetic organic hydrotalcite.(3 aminopropyl) triethoxysilane, salicylide and cobaltous chloride are made formation solution by the amount of 1:1:1 (mol ratio), adds magnetic organic hydrotalcite, form the organic coordination compound pillared hydrotalcite Han cobalt；To contain cobalt organic coordination compound pillared hydrotalcite to be placed in Muffle furnace, roasting 6～8h at 400～550 DEG C, the cycling of elements such as carbon nitrogen therein is gas overflowing, forms duct, obtains magnetic synergistic oxidation Co catalysts.This structure is conducive to absorption to be also catalyzed pollutant, is conducive to separating simultaneously.
Description
Technical field
The present invention relates to the exploitation of novel environmental pollution control material, particularly relate to a kind of magnetic synergistic oxidation Co catalysts
Preparation method.
Background technology
Hydrotalcite-based compound (LDHs) is the compound piled up by interlayer anion and positively charged laminate.Neatly
Stone chemical structure of general formula is: [M2+ 1-xM3+x(OH)2]x+[(An-)x/n·mH2O], wherein M2+And M3+Respectively it is positioned at main body laminate
On bivalence and trivalent metal cation, such as Mg2+、Ni2+、Zn2+、Mn2+、Cu2+、Co2+、Pd2+、Fe2+Deng bivalent cation and Al3 +、Cr3+、Co3+、Fe3+Brucite all can be formed Deng Tricationic；An–For interlayer anion, inorganic anion can be included,
Organic anion, coordination compound anion, same many and heteropolyanion；X is M3+/(M2++M3+) molar ratio, about 4:1 arrives
2:1；M is the number of intermediary water molecule.It is similar to that shepardite Mg (OH)2, octahedron share seamed edge and form main body
Laminate.The divalent metal M being positioned on laminate2+Can in certain proportion by ion half price close trivalent gold
Belong to cation M3+Isomorphous substitution so that laminate is positively charged, interlayer exist can exchange anion and laminate on positive electricity
Lotus balances so that the overall structure of LDHs is electric neutrality.The anion of interlayer can be exchanged, through a series of modifications, brucite
Material can obtain many materials planting different properties.
By modes such as ion exchanges, some compounds are introduced interlamination region, form the other pillar of molecular level, made
Class aperture is big, the horizontal composite of novel molecular of distribution rule, has absorption, the feature of conversion organic molecule.Brucite product
Kind many, the adjustability of pillar compound, modified clay material pore size, adsorption property etc. can artificially be controlled by,
Therefore can carry out material according to the difference of purposes to prepare, be widely used at the numerous areas such as petrochemical industry, environmental conservation
Prospect.
Cobalt oxide catalyst application is relatively wide, and such as ethylene and water gas, under Co catalysts effect, can obtain aldehyde and alcohol,
Novel co-based fischer-tropsch catalyst can be used for closing longer chain hydrocarbons and clear energy sources (Chem.Rev.2007,107,1692-1744), negative
Load type Co catalysts promote unsaturated fatty acid ester in double bond peroxidating (Xiamen University's journal (natural science edition), 2010
Year, volume 49,03 phase, 373-380), with Al (OH) x cobalt oxide catalyst as carrier, under conditions of not using a large amount of solvent
Carry out hexamethylene and toluene selective oxidation, achieve good result (catalysis journal, volume 2004,25,11 phases, 887-891).Separately
External catalysis aoxidizes the pollutant aspect of some difficult degradations, also has preferable application prospect, such as: at room temperature catalysis oxidation first
The Organic substance such as aldehyde, catalytic oxidation of cyclohexane (Catal.Commun.2005,6,211-214).But there is no the feelings of suitable carrier
Under condition, the efficiency of cobalt oxide is low；Have research CNT or mesopore silicon oxide (petroleum journal (PETROLEUM PROCESSING), 2011 01
Phase, chemistry journal, 16 phases in 2008), but these material prices are relatively costly.It addition, the active force between catalyst and carrier
How, also influence whether catalytic effect, cross weak, there will be catalyst and come off or be adsorbed in carrier cavity.After catalytic action
Exist separate difficulty problem, if to be separated totally, need, through multiple steps, to waste time and energy.
Summary of the invention
It is an object of the invention to as overcoming the deficiency that in prior art, cobalt oxide structure is single, it is provided that a kind of magnetic works in coordination with oxygen
Change the preparation method of Co catalysts.
The technical solution used in the present invention is in turn include the following steps:
1) by FeCl2It is dissolved in water, is configured to the solution that concentration is 2～3mol/L, take this solution of 500mL, will wherein
It is placed in constant temperature 70～80 DEG C of water-baths, is simultaneously added dropwise 30% (mass fraction) hydrogen peroxide 2～4mL and a certain amount of NaOH dilute molten
Liquid, keep pH value be 12～13, react 2～3h, proceed in autoclave, in 1h, be warmed up to 150～180 DEG C, continue reaction 4～
8h, naturally cools to room temperature, forms the precipitation with layer structure, precipitate and separate in this process, and deionization is washed 2～3 times；
2) solid that precipitation obtains is joined in the dodecylbenzene sodium sulfonate solution that concentration is 2～4mol/L, solid-liquid
Than be 1:10～1:50, be washed with deionized after 50～80 DEG C of stirred in water bath 2～8h, magnetic field separation 2～3 times, 70～
90 DEG C of drying, obtain magnetic organic hydrotalcite.
3) (3-aminopropyl) triethoxysilane, salicylide and cobaltous chloride are pressed 1:1:1 (mol ratio) amount each 2～
4mol joins formation solution in 20～40mL ethanol, reacts 6～8h, add magnetic organic hydrotalcite, stir at 20～35 DEG C
Mix 2～4h, precipitate and separate, reaction generate containing cobalt organic coordination compound under distributional effects, form the organic coordination compound Han cobalt pillared
Brucite；
4) will contain cobalt organic coordination compound pillared hydrotalcite to be placed in Muffle furnace, at 400～550 DEG C, roasting 6～8h, therein
The cycling of elements such as carbon nitrogen are gas overflowing, form duct, obtain magnetic synergistic oxidation Co catalysts.
The invention have the advantage that the ferric iron that part ferrous ion is generated by hydrogen peroxide oxidation, divalent ion and generation
Trivalent ion in 70～80 DEG C of water-baths under the effect of alkali, produce magnetic co-precipitation, form lamella hydrotalcite structure, then at sheet
Inter layer exchange enters surfactant so that it is surface is changed into hydrophilic by hydrophobicity, implants corresponding cobalt compound, eventually passes
Calcining, the material such as burning-off C, N, obtain having magnetic porous oxidation cobalt material.Synergism is had between ferrum cobalt, can be preferably
Promote catalytic action.
Detailed description of the invention
3 embodiments of the present invention are provided further below:
Embodiment 1
By FeCl2It is dissolved in water, is configured to the solution that concentration is 3mol/L, take this solution of 500mL, will wherein be placed in perseverance
In 75 DEG C of water-baths of temperature, being simultaneously added dropwise 30% (mass fraction) hydrogen peroxide 3mL and a certain amount of NaOH weak solution, holding pH value is
13, react 3h, proceed in autoclave, in 1h, be warmed up to 180 DEG C, continue reaction 8h, naturally cool to room temperature, in this process
Forming the precipitation with layer structure, precipitate and separate, deionization is washed 3 times；Solid precipitation obtained joins concentration
In the dodecylbenzene sodium sulfonate solution of 3mol/L, solid-to-liquid ratio is 1:20,80 DEG C of stirred in water bath 8h, spends after magnetic field separation
Ionized water washs 3 times, and 90 DEG C of drying obtain magnetic organic hydrotalcite.By (3-aminopropyl) triethoxysilane, salicylide and
Cobaltous chloride joins formation solution in 40mL ethanol by each 4mol of amount of 1:1:1 (mol ratio), reacts 8h, add magnetic at 35 DEG C
Property organic hydrotalcite, stir 4h, precipitate and separate, reaction generate containing cobalt organic coordination compound under distributional effects, formed and have containing cobalt
Machine coordination compound pillared hydrotalcite；Cobalt organic coordination compound pillared hydrotalcite will be contained be placed in Muffle furnace, roasting 7h at 550 DEG C, wherein
The cycling of elements such as carbon nitrogen be gas overflowing, form duct, obtain magnetic synergistic oxidation Co catalysts.
U-tube (internal diameter 4mm) flowing reactive evaluating apparatus continuously, the magnetic that weighing 100mg synthesis obtains is used to work in coordination with oxygen
Changing Co catalysts to place in pipe, and arrange a magnetic field at the mouth of pipe, the flow velocity of regulation air is 20mL/min, and air flowing drives
Formaldehyde gas enters in U-tube reactor, and the gas volume (i.e. air speed) flowing through every liter of catalyst per hour is 6000h-1.30
Under the conditions of DEG C, this catalyst degradation concentration is the formaldehyde gas of 200ppm, and degradation rate is 80.1%.
Embodiment 2
By FeCl2It is dissolved in water, is configured to the solution that concentration is 3mol/L, take this solution of 500mL, will wherein be placed in perseverance
In 80 DEG C of water-baths of temperature, being simultaneously added dropwise 30% (mass fraction) hydrogen peroxide 4mL and a certain amount of NaOH weak solution, holding pH value is
13, react 3h, proceed in autoclave, in 1h, be warmed up to 180 DEG C, continue reaction 8h, naturally cool to room temperature, in this process
Forming the precipitation with layer structure, precipitate and separate, deionization is washed 3 times；Solid precipitation obtained joins concentration
In the dodecylbenzene sodium sulfonate solution of 4mol/L, solid-to-liquid ratio is 1:50,80 DEG C of stirred in water bath 8h, spends after magnetic field separation
Ionized water washs 3 times, and 90 DEG C of drying obtain magnetic organic hydrotalcite.By (3-aminopropyl) triethoxysilane, salicylide and
Cobaltous chloride joins formation solution in 40mL ethanol by each 4mol of amount of 1:1:1 (mol ratio), reacts 8h, add magnetic at 35 DEG C
Property organic hydrotalcite, stir 4h, precipitate and separate, reaction generate containing cobalt organic coordination compound under distributional effects, formed and have containing cobalt
Machine coordination compound pillared hydrotalcite；Cobalt organic coordination compound pillared hydrotalcite will be contained be placed in Muffle furnace, roasting 8h at 550 DEG C, wherein
The cycling of elements such as carbon nitrogen be gas overflowing, form duct, obtain magnetic synergistic oxidation Co catalysts.
U-tube (internal diameter 4mm) flowing reactive evaluating apparatus continuously, the magnetic that weighing 100mg synthesis obtains is used to work in coordination with oxygen
Changing Co catalysts to place in pipe, and arrange a magnetic field at the mouth of pipe, the flow velocity of regulation air is 20mL/min, and air flowing drives
Formaldehyde gas enters in U-tube reactor, and the gas volume (i.e. air speed) flowing through every liter of catalyst per hour is 6000h-1.30
Under the conditions of DEG C, this catalyst degradation concentration is the formaldehyde gas of 200ppm, and degradation rate is 82.1%.
Embodiment 3
By FeCl2It is dissolved in water, is configured to the solution that concentration is 2mol/L, take this solution of 500mL, will wherein be placed in perseverance
In 70 DEG C of water-baths of temperature, being simultaneously added dropwise 30% (mass fraction) hydrogen peroxide 2mL and a certain amount of NaOH weak solution, holding pH value is
12, react 2h, proceed in autoclave, in 1h, be warmed up to 150 DEG C, continue reaction 4h, naturally cool to room temperature, in this process
Forming the precipitation with layer structure, precipitate and separate, deionization is washed 2 times；Solid precipitation obtained joins concentration
In the dodecylbenzene sodium sulfonate solution of 2mol/L, solid-to-liquid ratio is 1:10,50 DEG C of stirred in water bath 2h, spends after magnetic field separation
Ionized water washs 2 times, and 70 DEG C of drying obtain magnetic organic hydrotalcite.By (3-aminopropyl) triethoxysilane, salicylide and
Cobaltous chloride joins formation solution in 20mL ethanol by each 2mol of amount of 1:1:1 (mol ratio), reacts 6h, add magnetic at 20 DEG C
Property organic hydrotalcite, stir 2h, precipitate and separate, reaction generate containing cobalt organic coordination compound under distributional effects, formed and have containing cobalt
Machine coordination compound pillared hydrotalcite；Cobalt organic coordination compound pillared hydrotalcite will be contained be placed in Muffle furnace, roasting 6h at 400 DEG C, wherein
The cycling of elements such as carbon nitrogen be gas overflowing, form duct, obtain magnetic synergistic oxidation Co catalysts.
U-tube (internal diameter 4mm) flowing reactive evaluating apparatus continuously, the magnetic that weighing 100mg synthesis obtains is used to work in coordination with oxygen
Changing Co catalysts to place in pipe, and arrange a magnetic field at the mouth of pipe, the flow velocity of regulation air is 20mL/min, and air flowing drives
Formaldehyde gas enters in U-tube reactor, and the gas volume (i.e. air speed) flowing through every liter of catalyst per hour is 6000h-1.30
Under the conditions of DEG C, this catalyst degradation concentration is the formaldehyde gas of 200ppm, and degradation rate is 83.5%.
Claims (1)
1. a preparation method for magnetic synergistic oxidation Co catalysts, is characterized in that in turn including the following steps:
1) by FeCl2It is dissolved in water, is configured to the solution that concentration is 2～3mol/L, take this solution of 500mL, will wherein be placed in perseverance
In 70～80 DEG C of water-baths of temperature, it is simultaneously added dropwise 30% (mass fraction) hydrogen peroxide 2～4mL and a certain amount of NaOH weak solution, keeps
PH value is 12～13, reacts 2～3h, proceeds in autoclave, be warmed up to 150～180 DEG C in 1h, continues reaction 4～8h, natural
Being cooled to room temperature, form the precipitation with layer structure, precipitate and separate in this process, deionization is washed 2～3 times；
2) being joined by the solid that precipitation obtains in the dodecylbenzene sodium sulfonate solution that concentration is 2～4mol/L, solid-to-liquid ratio is
1:10～1:50, in 50～80 DEG C of stirred in water bath 2～8h, is washed with deionized 2～3 times after magnetic field separation, 70～90 DEG C
Dry, obtain magnetic organic hydrotalcite.
3) (3-aminopropyl) triethoxysilane, salicylide and cobaltous chloride are added by the amount each 2～4mol of 1:1:1 (mol ratio)
Enter in 20～40mL ethanol formation solution, at 20～35 DEG C react 6～8h, add magnetic organic hydrotalcite, stirring 2～
4h, precipitate and separate, reaction generate containing cobalt organic coordination compound under distributional effects, formed the pillared neatly of the organic coordination compound Han cobalt
Stone；
4) cobalt organic coordination compound pillared hydrotalcite will be contained be placed in Muffle furnace, roasting 6～8h at 400～550 DEG C, carbon nitrogen therein
It is gas overflowing Deng cycling of elements, forms duct, obtain magnetic synergistic oxidation Co catalysts.
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| CN109316920A (en) * | 2018-10-17 | 2019-02-12 | 厦门大学 | A kind of catalyst of transition metal oxide, preparation method and applications |
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| US6323367B1 (en) * | 2000-11-22 | 2001-11-27 | Council Of Scientific And Industrial Research | Process for the preparation of amine oxides |
| CN101780985A (en) * | 2010-01-26 | 2010-07-21 | 苏州科技学院 | Hydrotalcite-like compound used for raw water treatment |
| CN103769037A (en) * | 2014-02-27 | 2014-05-07 | 南京农业大学 | Preparation method of roasted ferro-manganese hydrotalcite and application of roasted ferro-manganese hydrotalcite in adsorption of arsenic-polluted wastewater |
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| US6323367B1 (en) * | 2000-11-22 | 2001-11-27 | Council Of Scientific And Industrial Research | Process for the preparation of amine oxides |
| CN101780985A (en) * | 2010-01-26 | 2010-07-21 | 苏州科技学院 | Hydrotalcite-like compound used for raw water treatment |
| CN103769037A (en) * | 2014-02-27 | 2014-05-07 | 南京农业大学 | Preparation method of roasted ferro-manganese hydrotalcite and application of roasted ferro-manganese hydrotalcite in adsorption of arsenic-polluted wastewater |
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| CN109316920A (en) * | 2018-10-17 | 2019-02-12 | 厦门大学 | A kind of catalyst of transition metal oxide, preparation method and applications |
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