CN105964262B - A kind of preparation method of magnetic coupling nickel oxide catalyst - Google Patents
A kind of preparation method of magnetic coupling nickel oxide catalyst Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 17
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 230000008878 coupling Effects 0.000 title claims abstract description 14
- 238000010168 coupling process Methods 0.000 title claims abstract description 14
- 238000005859 coupling reaction Methods 0.000 title claims abstract description 14
- 229910000480 nickel oxide Inorganic materials 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 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 29
- 229910001701 hydrotalcite Inorganic materials 0.000 claims abstract description 28
- 229960001545 hydrotalcite Drugs 0.000 claims abstract description 28
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 18
- 150000001875 compounds Chemical class 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000007789 gas Substances 0.000 claims abstract description 16
- MHAJPDPJQMAIIY-UHFFFAOYSA-N hydrogen peroxide Substances OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 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
- 230000001351 cycling effect Effects 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 5
- LAIZPRYFQUWUBN-UHFFFAOYSA-L nickel chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Ni+2] LAIZPRYFQUWUBN-UHFFFAOYSA-L 0.000 claims abstract description 3
- 238000001556 precipitation Methods 0.000 claims description 20
- 238000000926 separation method Methods 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000002242 deionisation method Methods 0.000 claims description 8
- 230000000694 effects Effects 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 235000019441 ethanol Nutrition 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- 230000003647 oxidation Effects 0.000 abstract description 6
- 238000007254 oxidation reaction Methods 0.000 abstract description 6
- 239000007868 Raney catalyst Substances 0.000 abstract description 5
- 229910000564 Raney nickel Inorganic materials 0.000 abstract description 5
- 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
- 230000002195 synergetic effect Effects 0.000 abstract description 2
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 abstract 1
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 abstract 1
- 239000013049 sediment Substances 0.000 abstract 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 18
- 239000000463 material Substances 0.000 description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- 230000015556 catabolic process Effects 0.000 description 6
- 238000006731 degradation reaction Methods 0.000 description 6
- 239000011229 interlayer Substances 0.000 description 6
- 150000001450 anions Chemical class 0.000 description 5
- 239000010410 layer Substances 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 150000001768 cations Chemical class 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000005406 washing 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
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-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
- 238000009825 accumulation Methods 0.000 description 1
- 230000009471 action Effects 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
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 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
- 229910001412 inorganic anion Inorganic materials 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- UGKDIUIOSMUOAW-UHFFFAOYSA-N iron nickel Chemical compound [Fe].[Ni] UGKDIUIOSMUOAW-UHFFFAOYSA-N 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002121 nanofiber Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 150000002816 nickel compounds Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 150000002891 organic anions Chemical class 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000004224 protection Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 230000010148 water-pollination Effects 0.000 description 1
- 229910003158 γ-Al2O3 Inorganic materials 0.000 description 1
Classifications
-
- B01J35/33—
-
- 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
- B01J23/755—Nickel
Abstract
The present invention discloses a kind of preparation method of magnetic coupling nickel oxide catalyst.It in turn includes the following steps：Under the conditions of water bath with thermostatic control, FeCl2Hydrogen peroxide and NaOH weak solutions are added dropwise in solution, is transferred in autoclave after stirring, the reaction was continued, naturally cools to room temperature, obtains solid sediment, adds it in neopelex solution, obtains magnetic organic hydrotalcite.By (3 aminopropyl) triethoxysilane, salicylide and Nickel dichloride hexahydrate in molar ratio 1：1：1 amount is made to form solution, adds in magnetic organic hydrotalcite, forms nickeliferous organic coordination compound pillared hydrotalcite；Nickeliferous organic coordination compound pillared hydrotalcite is placed in Muffle furnace, it is gas overflowing that the cycling of elements such as 6~8h, carbon nitrogen therein are roasted at 400~550 DEG C, forms duct, obtains magnetic synergistic oxidation Raney nickel.The structure is conducive to absorption and is also catalyzed pollutant, while be conducive to detach.
Description
Technical field
Exploitation more particularly to a kind of magnetic coupling nickel oxide catalyst the present invention relates to novel environmental pollution control material
Preparation method.
Background technology
Hydrotalcite-based compound (LDHs) is the compound formed by interlayer anion and the accumulation of 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 located at main layer board
On divalent and trivalent metal cation, such as Mg2+、Ni2+、Zn2+、Mn2+、Cu2+、Co2+、Pd2+、Fe2+Wait bivalent cations and Al3 +、Cr3+、Co3+、Fe3+Wait Tricationics that can form hydrotalcite；An–For interlayer anion, inorganic anion can be included,
Organic anion, complex anion, with mostly and heteropolyanion；X is M3+/(M2++M3+) molar ratio, about 4:1 arrives
2:1；M is the number of interlayer hydrone.Its structure is similar to shepardite Mg (OH)2, main body is formed by the shared seamed edge of octahedron
Laminate.Divalent metal M on laminate2+Can in a certain proportion similar in ion half price trivalent gold
Belong to cation M3+Same order elements so that laminate is positively charged, and interlayer has the positive electricity on the anion and laminate that can be exchanged
Lotus balances so that the overall structure of LDHs is in electroneutral.The anion of interlayer can be exchanged, by a series of modifications, hydrotalcite
Material can obtain the substance of many kinds of different properties.
By the modes such as ion exchange some compounds introduce interlamination region, formed the other pillar of molecular level, manufactured one
Class aperture is big, the horizontal composite material of novel molecular of distribution rule, has the characteristics that absorption, conversion organic molecule.Hydrotalcite product
Kind of more, the adjustability of pillar compound, modified clay material pore size, adsorption property etc. can taking human as being controlled,
Therefore can material preparation be carried out according to the difference of purposes, be widely used in numerous areas such as petrochemical industry, environmental protections
Prospect.
Transition metal oxide has excellent electrical and optical properties mostly, also with excellent catalytic performance.Nanometer
Nickel oxide is a kind of important functional material, due to size and the uniqueness of pattern, is inhaled in covering with paint, catalysis, capacitance electrode, light
Important application is suffered from the industrial circles such as receipts, gas sensing.It is required according to the pattern to nano material is different from size,
People have prepared the nano particle of nickel oxide, nanometer rods, nano wire, nanofiber, nanometer sheet using various methods.But nanometer
Material is having the shortcomings that its is intrinsic i.e. during use：Easily reunite, it is therefore desirable to be carried on carrier surface to obtain most
Good using effect.
Nickel oxide catalyst application is wider, before also having preferable application in terms of some pollutants difficult to degrade in catalysis oxidation
Scape, such as：The organic matters such as catalysis oxidation formaldehyde, catalytic oxidation of cyclohexane at room temperature.But no suitable carrier, nickel oxide
Dosage is big, and efficiency is low；There are research carbon nanotube or γ-Al2O3, but these material prices are relatively expensive.
There is the problem of separation is difficult after catalytic action, if to be separated clean, need by multiple steps, it is time-consuming to take
Power.
Invention content
The purpose of the present invention is to overcome the shortcomings of that nickel oxide structure is single in the prior art, provide a kind of magnetic coupling oxygen
Change the preparation method of Raney nickel.
The technical solution adopted by the present invention is in turn include the following steps：
1) by FeCl2It is dissolved into water, is configured to the solution of a concentration of 2~3mol/L, take the 500mL solution, it will wherein
It is placed in 70~80 DEG C of water-baths of constant temperature, while 2~4mL of hydrogen peroxide and a certain amount of NaOH that mass fraction 30% is added dropwise are dilute molten
Liquid, it is 12~13 to keep pH value, reacts 2~3h, is transferred in autoclave, 150~180 DEG C are warming up in 1h, the reaction was continued 4~
8h naturally cools to room temperature, forms the precipitation with layer structure, precipitation separation in this process, and deionization is washed 2~3 times；
2) solid that precipitation obtains is added in the neopelex solution of a concentration of 2~4mol/L, solid-liquid
Than being 1：10~1：50, in 50~80 DEG C of 2~8h of stirred in water bath, it is washed with deionized 2~3 times after the separation of magnetic field, 70~
90 DEG C of drying, obtain magnetic organic hydrotalcite.
3) by (3- aminopropyls) triethoxysilane, salicylide and Nickel dichloride hexahydrate in molar ratio 1：1：1 amount each 2
~4mol is added in 20~40mL ethyl alcohol and forms solution, and 6~8h is reacted at 20~35 DEG C, adds in magnetic organic hydrotalcite,
2~4h, precipitation separation are stirred, the nickeliferous organic coordination compound of generation is reacted under distributional effects, forms nickeliferous organic coordination compound column
Support hydrotalcite；
4) nickeliferous organic coordination compound pillared hydrotalcite is placed in Muffle furnace, 6~8h is roasted at 400~550 DEG C, it is therein
The cycling of elements such as carbon nitrogen are gas overflowing, form duct, obtain magnetic coupling nickel oxide catalyst.
It is an advantage of the invention 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 action of alkali, generate magnetic co-precipitation, form lamella hydrotalcite structure, then in piece
Inter layer exchange enters surfactant, its surface is made to be changed into hydrophily by hydrophobicity, is implanted into corresponding nickel compound, finally passes through
The substances such as calcining, burning-off C, N, obtain having magnetic porous oxidation nickel material.Iron nickel adulterates, synergistic effect, promotes catalysis effect
Fruit.
Specific embodiment
3 embodiments of the present invention are provided further below：
Embodiment 1
By FeCl2It is dissolved into water, is configured to the solution of a concentration of 3mol/L, take the 500mL solution, will wherein be placed in perseverance
In warm 75 DEG C of water-baths, while 30% hydrogen peroxide 3mL of mass fraction and a certain amount of NaOH weak solutions is added dropwise, it is 13 to keep pH value,
3h is reacted, is transferred in autoclave, 180 DEG C is warming up in 1h, the reaction was continued 8h naturally cools to room temperature, in this process shape
Into the precipitation with layer structure, precipitation separation, deionization is washed 3 times；The solid that precipitation obtains is added to a concentration of 3mol/
In the neopelex solution of L, solid-to-liquid ratio 1：20, use deionization after 80 DEG C of stirred in water bath 8h, magnetic field separation
Water washing 3 times, 90 DEG C of drying, obtains magnetic organic hydrotalcite.By (3- aminopropyls) triethoxysilane, salicylide and six water
Close nickel chloride in molar ratio 1：1：1 each 4mol of amount, which is added in 40mL ethyl alcohol, forms solution, and 8h is reacted at 35 DEG C, adds in magnetic
Property organic hydrotalcite, stirring 4h, precipitation separation react the nickeliferous organic coordination compound of generation under distributional effects, and being formed nickeliferous has
Machine complex pillared hydrotalcite；Nickeliferous organic coordination compound pillared hydrotalcite is placed in Muffle furnace, 7h is roasted at 550 DEG C, wherein
The cycling of elements such as carbon nitrogen be gas overflowing, form duct, obtain magnetic coupling nickel oxide catalyst.
Reaction evaluating device is continuously flowed using U-tube (internal diameter 4mm), weighs the magnetic coupling oxygen that 100mg is synthesized
Change Raney nickel to place in pipe, and a magnetic field is set at nozzle, the flow velocity for adjusting air is 20mL/min, and air flowing drives
Formaldehyde gas enters in U-tube reactor, and the gas volume (i.e. air speed) for flowing through every liter of catalyst per hour is 6000h-1.30
Under the conditions of DEG C, the formaldehyde gas of a concentration of 200ppm of the catalyst degradation, degradation rate 82.5%.
Embodiment 2
By FeCl2It is dissolved into water, is configured to the solution of a concentration of 3mol/L, take the 500mL solution, will wherein be placed in perseverance
In warm 80 DEG C of water-baths, while 30% hydrogen peroxide 4mL of mass fraction and a certain amount of NaOH weak solutions is added dropwise, it is 13 to keep pH value,
3h is reacted, is transferred in autoclave, 180 DEG C is warming up in 1h, the reaction was continued 8h naturally cools to room temperature, in this process shape
Into the precipitation with layer structure, precipitation separation, deionization is washed 3 times；The solid that precipitation obtains is added to a concentration of 4mol/
In the neopelex solution of L, solid-to-liquid ratio 1：50, use deionization after 80 DEG C of stirred in water bath 8h, magnetic field separation
Water washing 3 times, 90 DEG C of drying, obtains magnetic organic hydrotalcite.By (3- aminopropyls) triethoxysilane, salicylide and six water
Close nickel chloride in molar ratio 1：1：1 each 4mol of amount, which is added in 40mL ethyl alcohol, forms solution, and 8h is reacted at 35 DEG C, adds in magnetic
Property organic hydrotalcite, stirring 4h, precipitation separation react the nickeliferous organic coordination compound of generation under distributional effects, and being formed nickeliferous has
Machine complex pillared hydrotalcite；Nickeliferous organic coordination compound pillared hydrotalcite is placed in Muffle furnace, 8h is roasted at 550 DEG C, wherein
The cycling of elements such as carbon nitrogen be gas overflowing, form duct, obtain magnetic coupling nickel oxide catalyst.
Reaction evaluating device is continuously flowed using U-tube (internal diameter 4mm), weighs the magnetic coupling oxygen that 100mg is synthesized
Change Raney nickel to place in pipe, and a magnetic field is set at nozzle, the flow velocity for adjusting air is 20mL/min, and air flowing drives
Formaldehyde gas enters in U-tube reactor, and the gas volume (i.e. air speed) for flowing through every liter of catalyst per hour is 6000h-1.30
Under the conditions of DEG C, the formaldehyde gas of a concentration of 200ppm of the catalyst degradation, degradation rate 81.5%.
Embodiment 3
By FeCl2It is dissolved into water, is configured to the solution of a concentration of 2mol/L, take the 500mL solution, will wherein be placed in perseverance
In warm 70 DEG C of water-baths, while 30% hydrogen peroxide 2mL of mass fraction and a certain amount of NaOH weak solutions is added dropwise, it is 12 to keep pH value,
2h is reacted, is transferred in autoclave, 150 DEG C is warming up in 1h, the reaction was continued 4h naturally cools to room temperature, in this process shape
Into the precipitation with layer structure, precipitation separation, deionization is washed 2 times；The solid that precipitation obtains is added to a concentration of 2mol/
In the neopelex solution of L, solid-to-liquid ratio 1：10, use deionization after 50 DEG C of stirred in water bath 2h, magnetic field separation
Water washing 2 times, 70 DEG C of drying, obtains magnetic organic hydrotalcite.By (3- aminopropyls) triethoxysilane, salicylide and six water
Close nickel chloride in molar ratio 1：1：1 each 2mol of amount, which is added in 20mL ethyl alcohol, forms solution, and 6h is reacted at 20 DEG C, adds in magnetic
Property organic hydrotalcite, stirring 2h, precipitation separation react the nickeliferous organic coordination compound of generation under distributional effects, and being formed nickeliferous has
Machine complex pillared hydrotalcite；Nickeliferous organic coordination compound pillared hydrotalcite is placed in Muffle furnace, 6h is roasted at 400 DEG C, wherein
The cycling of elements such as carbon nitrogen be gas overflowing, form duct, obtain magnetic coupling nickel oxide catalyst.
Reaction evaluating device is continuously flowed using U-tube (internal diameter 4mm), weighs the magnetic coupling oxygen that 100mg is synthesized
Change Raney nickel to place in pipe, and a magnetic field is set at nozzle, the flow velocity for adjusting air is 20mL/min, and air flowing drives
Formaldehyde gas enters in U-tube reactor, and the gas volume (i.e. air speed) for flowing through every liter of catalyst per hour is 6000h-1.30
Under the conditions of DEG C, the formaldehyde gas of a concentration of 200ppm of the catalyst degradation, degradation rate 82.7%.
Claims (1)
1. a kind of preparation method of magnetic coupling nickel oxide catalyst, it is characterized in that in turn including the following steps：
1) by FeCl2It is dissolved into water, is configured to the solution of a concentration of 2~3mol/L, take the 500mL solution, will wherein be placed in perseverance
In warm 70~80 DEG C of water-baths, while 2~4mL of hydrogen peroxide of mass fraction 30% and a certain amount of NaOH weak solutions is added dropwise, keeps
PH value is 12~13, reacts 2~3h, is transferred in autoclave, 150~180 DEG C are warming up in 1h, and the reaction was continued 4~8h is natural
Room temperature is cooled to, forms the precipitation with layer structure, precipitation separation in this process, deionization is washed 2~3 times；
2) solid that precipitation obtains is added in the neopelex solution of a concentration of 2~4mol/L, solid-to-liquid ratio is
1：10~1：50, it is washed with deionized 2~3 times, 70~90 DEG C after 50~80 DEG C of 2~8h of stirred in water bath, magnetic field separation
Drying, obtains magnetic organic hydrotalcite；
3) by (3- aminopropyls) triethoxysilane, salicylide and Nickel dichloride hexahydrate in molar ratio 1：1：1 amount each 2~
4mol is added in 20~40mL ethyl alcohol and forms solution, and 6~8h is reacted at 20~35 DEG C, adds in magnetic organic hydrotalcite, stirs
2~4h, precipitation separation are mixed, the nickeliferous organic coordination compound of generation is reacted under distributional effects, it is pillared to form nickeliferous organic coordination compound
Hydrotalcite；
4) nickeliferous organic coordination compound pillared hydrotalcite is placed in Muffle furnace, 6~8h, carbon nitrogen therein is roasted at 400~550 DEG C
It is gas overflowing to wait cycling of elements, forms duct, obtains magnetic coupling nickel oxide catalyst.
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| CN106621774A (en) * | 2017-01-20 | 2017-05-10 | 杭州启澄科技有限公司 | Treatment method for purifying industrial waste gas |
| CN110282666A (en) * | 2019-07-22 | 2019-09-27 | 辽宁科技大学 | A kind of nickel-ferric spinel and its preparation method and application |
| CN111229232B (en) * | 2020-03-20 | 2023-10-31 | 苏州大学 | Foam nickel-based porous NiFe hydrotalcite nano-sheet and preparation and application thereof |
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| 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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2016
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