CN106179352B - A kind of Ni-based nano particle catalysis material of multiphase metatitanic acid and preparation method thereof - Google Patents
A kind of Ni-based nano particle catalysis material of multiphase metatitanic acid and preparation method thereof Download PDFInfo
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- 239000002253 acid Substances 0.000 title claims abstract description 49
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 41
- 239000000463 material Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000006555 catalytic reaction Methods 0.000 title claims abstract description 15
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 75
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 24
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 17
- DGXKDBWJDQHNCI-UHFFFAOYSA-N dioxido(oxo)titanium nickel(2+) Chemical compound [Ni++].[O-][Ti]([O-])=O DGXKDBWJDQHNCI-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000010936 titanium Substances 0.000 claims abstract description 17
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 235000019441 ethanol Nutrition 0.000 claims abstract description 8
- 230000005291 magnetic effect Effects 0.000 claims abstract description 6
- 230000001699 photocatalysis Effects 0.000 claims abstract description 5
- 238000007146 photocatalysis Methods 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims abstract description 3
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical group [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 9
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical group CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 5
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 2
- 229940078494 nickel acetate Drugs 0.000 claims description 2
- 150000002148 esters Chemical class 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- 238000001354 calcination Methods 0.000 description 13
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 10
- 238000006731 degradation reaction Methods 0.000 description 9
- XIKYYQJBTPYKSG-UHFFFAOYSA-N nickel Chemical compound [Ni].[Ni] XIKYYQJBTPYKSG-UHFFFAOYSA-N 0.000 description 9
- 229910000480 nickel oxide Inorganic materials 0.000 description 9
- 230000015556 catabolic process Effects 0.000 description 8
- 239000013078 crystal Substances 0.000 description 8
- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 description 8
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 5
- 235000013339 cereals Nutrition 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 235000003283 Pachira macrocarpa Nutrition 0.000 description 3
- 241001083492 Trapa Species 0.000 description 3
- 235000014364 Trapa natans Nutrition 0.000 description 3
- 235000009165 saligot Nutrition 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 239000003403 water pollutant Substances 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000005290 antiferromagnetic effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
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- 238000007716 flux method Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 description 1
- 239000011807 nanoball Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 125000000636 p-nitrophenyl group Chemical group [H]C1=C([H])C(=C([H])C([H])=C1*)[N+]([O-])=O 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- AGGKEGLBGGJEBZ-UHFFFAOYSA-N tetramethylenedisulfotetramine Chemical compound C1N(S2(=O)=O)CN3S(=O)(=O)N1CN2C3 AGGKEGLBGGJEBZ-UHFFFAOYSA-N 0.000 description 1
- 238000003911 water pollution 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
- B01J23/70—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
-
- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- 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
- B01J35/39—Photocatalytic properties
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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
Abstract
The invention belongs to energy and material manufacturing technology fields, and in particular to a kind of multiphase metatitanic acid Ni-based nano particle catalysis material and preparation method thereof.The preparation method is that: nickel source, ethyl alcohol and acid are uniformly mixed, 30~60min of stirring in constant temperature blender with magnetic force is placed in；It is cooled to room temperature, titanium source is added, reacts nickel source and titanium source sufficiently, after reaction, is cooled to room temperature again, deionized water is then added, stir evenly；After acquired solution low temperature drying, the presoma of nickel titanate is obtained；After the presoma of gained nickel titanate is calcined, the Ni-based nano particle catalysis material of multiphase metatitanic acid is obtained.Using the Ni-based nanoparticle semiconductive catalysis material of multiphase metatitanic acid that one-step method of the present invention directly synthesizes there is growth to stablize, it is of uniform size, large specific surface area, the advantages that surface-active site is more, increase effectively the separation of photo-generated carrier, the rate of electron-transport is increased, sun light utilization efficiency is improved, photocatalysis performance is high.
Description
Technical field
The invention belongs to energy and material manufacturing technology fields, and in particular to a kind of multiphase metatitanic acid Ni-based nano particle light is urged
Change material and preparation method thereof.
Background technique
As the discharge of industrial wastewater inevitably enters water environment, cause water pollution, causes pollution water quality long-term
Deteriorate, seriously endangers human health.Therefore, research degradation water pollutant is the significant problem that countries in the world are faced.Cause
Sunlight is inexhaustible, therefore developing and using solar energy is the problem of people increasingly pay attention to, and seeks novel light
The problem of catalyst is researcher's extensive concern.It is ring in recent years using Photocatalytic Oxidation With Semiconductors technology degradation water pollutant
A research hotspot in the control of border, existing numerous studies prove numerous hardly degraded organic substances in the effect of photochemical catalytic oxidation
Under effectively can be able to remove or degrade.
Metatitanic acid nickel material is used as II B- of one kind, VI A race semiconducting compound, and forbidden bandwidth at room temperature is 2.8eV, has
Good electric conductivity and wider absorption wave range, are a kind of very promising catalysis materials, are expected to solving organic dyestuff
And to playing a significant role in the pollution problem of environment.According to the literature, pass through hydro-thermal method, sol-gal process, pass flux
Method, Pechini method, coprecipitation etc. prepare the nickel titanate of single-phase nanotube, nanometer rods.But prepared single-phase metatitanic acid
The compound probability of nickel photo-generated carrier is higher, is difficult to make full use of sunlight.
Nickel oxide is the P-type antiferromagnetic semiconducter functional material of forbidden bandwidth about 3.6eV a kind of, due to its extensive use
In fields such as gas sensor, catalyst, fuel cell electrode, optical activity fiber and magnetic materials, recently by scientific research work
The favor of author.Liu et al. (Liu L, Li Y, Yuan S M, J.Phys.Chem.C, 2010,114,251-255) utilizes six times
Tetramine has the nickel oxide nano ball of graded structure as additive synthesis.(Wei F, Wu Y F, the Luo L such as Wei Fei
H, [J] .Chinese Ceramic Society, 2009,37 (12): 1975-1981 (in Chinese)) use homogeneous precipitation
Method prepares the NiO nanometer sheet self-assembly of flower-like structure in methanol-water medium using urea and nickel nitrate as raw material, however,
They in an experiment involved in operating process complex (for example elapsed time is wanted to remove removing template) and easily increase experimental cost,
Consumptive material is caused to consume energy.Therefore, the pattern to NiO inorganic material, dimensional structure are realized using a kind of simple effective method
Design is constructed and regulated and controled, is still the key of research.
Summary of the invention
The present invention is for the deficiencies in the prior art, and it is an object of the present invention to provide a kind of multiphase metatitanic acid nickel-nickel oxide-dioxy
Change the nano particle catalysis material and preparation method thereof of titanium.
For achieving the above object, the technical scheme adopted by the invention is as follows:
A kind of preparation method of the Ni-based nano particle catalysis material of multiphase metatitanic acid, includes the following steps:
(1) nickel source, ethyl alcohol and acid are uniformly mixed, are placed in 30~60min of stirring in constant temperature blender with magnetic force；It is cooled to room
Temperature is added titanium source, reacts nickel source and titanium source sufficiently, after reaction, be cooled to room temperature again, deionized water is then added,
It stirs evenly；After acquired solution low temperature drying, the presoma of nickel titanate is obtained；
(2) it by after the presoma calcine by steps of nickel titanate obtained by step (1), obtains the Ni-based nano particle light of multiphase metatitanic acid and urges
Change material.
In above scheme, the molar ratio of the nickel source and titanium source is 1:1~2.
In above scheme, the volume ratio of the ethyl alcohol, acid and deionized water is 5:1:1~5:2:2.
In above scheme, the nickel source is nickel nitrate or nickel acetate.
In above scheme, the acid is nitric acid or acetic acid.
In above scheme, the titanium source is isopropyl titanate or tetrabutyl titanate.
In above scheme, the drying temperature of low temperature drying described in step (1) is 40~60 DEG C, drying time is 6~
20h。
In above scheme, the technique of calcine by steps described in step (2) are as follows: 200~300 DEG C, 2~3h；400~500 DEG C,
2~3h, 600~700 DEG C, 4~6h, heating rate is 2~5 DEG C/min.
The Ni-based nano particle catalysis material of the multiphase metatitanic acid that above-mentioned preparation method is prepared.
Beneficial effects of the present invention: (1) multiphase metatitanic acid nickel base nanometer is prepared using solution-calcination method in the present invention
Grain compares high-temperature calcination synthesis technology more in the prior art, and the multiphase metatitanic acid that preparation method of the present invention obtains is Ni-based to be received
Rice grain growth is more stable, and size is more uniform；Meanwhile also there is large specific surface area, the advantage more than surface-active site can be effective
The separation for increasing photo-generated carrier, increases the rate of electron-transport, improves the utilization rate of sunlight, photocatalysis performance is higher；(2)
The present invention has directly synthesized the Ni-based nanoparticle semiconductive catalysis material of multiphase metatitanic acid, the preparation method using one-step method
It is simple to operation.
Detailed description of the invention
Fig. 1 is the X-ray diffractogram of the Ni-based nano particle of multiphase metatitanic acid of the embodiment of the present invention 1,2,3.
Fig. 2 is multiphase nickel titanate-nickel oxide nanoparticle scanning electron microscope (SEM) image of the embodiment of the present invention 1.
Fig. 3 is multiphase metatitanic acid nickel-nickel oxide-titania nanoparticles scanning electron microscope of the embodiment of the present invention 2
Image.
Fig. 4 is multiphase metatitanic acid nickel-nickel oxide-titania nanoparticles scanning electron microscope of the embodiment of the present invention 3
Image.
Fig. 5 is the degradation rate of the photocatalytic degradation nitrobenzene of the Ni-based nano particle of multiphase metatitanic acid of preparation of the embodiment of the present invention
Figure.
Fig. 6 is the degradation speed of the photocatalytic degradation nitrobenzene of the Ni-based nano particle of multiphase metatitanic acid of preparation of the embodiment of the present invention
Rate figure.
Specific embodiment
For a better understanding of the present invention, below with reference to the embodiment content that the present invention is furture elucidated, but it is of the invention
Content is not limited solely to the following examples.
Embodiment 1
A kind of Ni-based nano particle catalysis material of multiphase metatitanic acid, is prepared via a method which to obtain:
(1) nickel nitrate of 0.016moL is dissolved in 10mL ethyl alcohol, is placed in 25 DEG C of constant temperature blender with magnetic force, 2mL is added
Concentrated nitric acid and be stirred continuously, be completely dissolved to nickel nitrate, continue 30~60min of stirring；
(2) step (1) acquired solution is cooled to room temperature, be added 0.0128moL isopropyl titanate (titanium source and nickel source
Molar ratio is 1.25:1)；
(3) it is cooled to room temperature to step (2) acquired solution, 2~4mL deionized water is added, stirs evenly；
(4) step (3) acquired solution is placed in drying in baking oven, temperature is controlled at 60 DEG C, and drying time 20h obtains titanium
The presoma of sour nickel；
(5) presoma of nickel titanate obtained by step (4) is placed in Muffle furnace and is calcined: 300 DEG C of calcining 2h, 400 DEG C of calcinings
2h, 650 DEG C of calcining 4h, heating rate are 2 DEG C/min, arrive the Ni-based nano particle of multiphase metatitanic acid after calcining.
The Ni-based nano particle X-ray diffractogram (XRD) of the multiphase metatitanic acid that the present embodiment is prepared as shown in Figure 1,
24.16 °, 33.13 °, 35.69 °, 40.89 °, 49.49 °, 54.03 °, 57.40 °, 62.50 °, 64.12 ° respectively correspond oblique water chestnut side
The nickel titanate (012) of crystallographic system, (104), (110), (113), (024), (116), (018), (214),
(300) crystal face.37.23 °, 43.29 ° respectively correspond (001) of nickel oxide, (200) crystal face, illustrate to have synthesized multiphase
The Ni-based nano particle of metatitanic acid be multiphase nickel titanate-nickel oxide nanoparticle, main phase is nickel titanate.
Multiphase nickel titanate-nickel oxide nanoparticle scanning electron microscope diagram that the present embodiment is prepared is shown in Fig. 2, by
Scanning figure finds out that multiphase nickel titanate-nickel oxide nanoparticle size is relatively stable, and the size of nano particle is 80nm or so.
Embodiment 2
A kind of Ni-based nano particle catalysis material of multiphase metatitanic acid, is prepared via a method which to obtain:
(1) nickel nitrate of 0.016moL is dissolved in 10mL ethyl alcohol, is placed in 25 DEG C of constant temperature blender with magnetic force, 2mL is added
Concentrated nitric acid and be stirred continuously, be completely dissolved to nickel nitrate, continue 30~60min of stirring；
(2) step (1) acquired solution is cooled to room temperature, be added 0.0154moL isopropyl titanate (titanium source and nickel source
Molar ratio is 1.04:1)；
(3) it is cooled to room temperature to step (2) acquired solution, 2~4mL deionized water is added, stirs evenly；
(4) step (3) acquired solution is placed in drying in baking oven, temperature is controlled at 60 DEG C, and drying time 18h obtains titanium
The presoma of sour nickel；
(5) presoma of nickel titanate obtained by step (4) is placed in Muffle furnace and is calcined: 300 DEG C of calcining 2h, 400 DEG C of calcinings
2h, 650 DEG C of calcining 4h, heating rate are 2 DEG C/min, arrive the Ni-based nano particle of multiphase metatitanic acid after calcining.
The Ni-based nano particle X-ray diffractogram (XRD) of the multiphase metatitanic acid that the present embodiment is prepared as shown in Figure 1,
24.16 °, 33.13 °, 35.69 °, 40.89 °, 49.49 °, 54.03 °, 57.40 °, 62.50 °, 64.12 ° respectively correspond oblique water chestnut side
Nickel titanate (012), (104), (110), (113), (024), (116), (018), (214), (300) crystal face of crystallographic system；37.23°,
43.29 ° respectively correspond (001) of nickel oxide, (200) crystal face；25.34 °, 48.10 ° (101) for respectively corresponding anatase,
(200) crystal face illustrates to have synthesized multiphase metatitanic acid nickel-nickel oxide-titania nanoparticles, and main phase is nickel titanate.
Multiphase metatitanic acid nickel-nickel oxide-titania nanoparticles scanning electron microscope that the present embodiment is prepared
Figure is shown in Fig. 3, finds out that multiphase metatitanic acid nickel-nickel oxide-titania nanoparticles size is relatively stable by scanning figure, nanometer
The size of grain is 80nm or so.
Embodiment 3
A kind of Ni-based nano particle catalysis material of multiphase metatitanic acid, is prepared via a method which to obtain:
(1) nickel nitrate of 0.016moL is dissolved in 10mL ethyl alcohol, is placed in 25 DEG C of constant temperature blender with magnetic force, 2mL is added
Concentrated nitric acid and be stirred continuously, be completely dissolved to nickel nitrate, continue 30~60min of stirring；
(2) step (1) acquired solution is cooled to room temperature, be added 0.016moL isopropyl titanate (titanium source and nickel source
Molar ratio is 1:1)；
(3) it is cooled to room temperature to step (2) acquired solution, 2~4mL deionized water is added, stirs evenly；
(4) step (3) acquired solution is placed in drying in baking oven, temperature is controlled at 40 DEG C, and drying time 20h obtains titanium
The presoma of sour nickel；
(5) presoma of nickel titanate obtained by step (4) is placed in Muffle furnace and is calcined: 300 DEG C of calcining 2h, 400 DEG C of calcinings
2h, 650 DEG C of calcining 4h, heating rate are 2 DEG C/min, arrive the Ni-based nano particle of metatitanic acid after calcining.
The Ni-based nano particle X-ray diffractogram (XRD) of the multiphase metatitanic acid that the present embodiment is prepared as shown in Figure 1,
24.16 °, 33.13 °, 35.69 °, 40.89 °, 49.49 °, 54.03 °, 57.40 °, 62.50 °, 64.12 ° respectively correspond oblique water chestnut side
Nickel titanate (012), (104), (110), (113), (024), (116), (018), (214), (300) crystal face of crystallographic system；37.23°,
43.29 ° respectively correspond (001) of nickel oxide, (200) crystal face；25.34 °, 48.10 ° (101) for respectively corresponding anatase,
(200) crystal face illustrates to have synthesized multiphase metatitanic acid nickel-nickel oxide-titania nanoparticles, and main phase is nickel titanate.
Multiphase metatitanic acid nickel-nickel oxide-titania nanoparticles scanning electron microscope that the present embodiment is prepared
Figure is shown in Fig. 4, finds out that multiphase metatitanic acid nickel-nickel oxide-titania nanoparticles size is relatively stable by scanning figure, nanometer
The size of grain is 80nm or so.
It is 50ppm that each 20mg of the Ni-based nano particle of multiphase metatitanic acid prepared by Example 1~3, which is respectively placed in 80mL concentration,
Nitro benzene aquatic solution in, darkroom stirring 1h reaches adsorption-desorption balance, under visible light illumination (luminous intensity are as follows: visible light portion
Divide 158mWcm-2), start to carry out degradation reaction, takes a sample every 60min, be centrifuged, measure nitrobenzene solution in each sample
Concentration C, with C/C0For ordinate, the reaction time is abscissa, draws degradation rate figure (as shown in Figure 5), will react degradation rate
It is depicted as degradation rate figure (as shown in Figure 6), from figs. 5 and 6, it can be seen that the present invention prepares gained multiphase metatitanic acid nickel base nanometer
The photocatalysis performance of particle is higher, and the degradation effect of p-nitrophenyl is preferable.
Obviously, above-described embodiment is only intended to clearly illustrate made example, and is not the limitation to embodiment.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And the obvious variation or change therefore amplified
It moves within still in the protection scope of the invention.
Claims (6)
1. a kind of preparation method of the Ni-based nano particle catalysis material of multiphase metatitanic acid, which comprises the steps of:
(1) nickel source, ethyl alcohol and acid are uniformly mixed, are placed in 30 ~ 60min of stirring in constant temperature blender with magnetic force；It is cooled to room temperature, adds
Enter titanium source, react nickel source and titanium source sufficiently, after reaction, be cooled to room temperature again, deionized water is then added, stirring is equal
It is even；After acquired solution low temperature drying, the presoma of nickel titanate is obtained；The molar ratio of the nickel source and titanium source is 1:1 ~ 2；It is described
The volume ratio of ethyl alcohol, acid and deionized water is 5:1:1 ~ 5:2:2；
(2) by after the presoma calcine by steps of nickel titanate obtained by step (1), the Ni-based nano particle photocatalysis material of multiphase metatitanic acid is obtained
Material；The technique of the calcine by steps are as follows: 200 ~ 300 DEG C, 2 ~ 3h；400 ~ 500 DEG C, 2 ~ 3h, 600 ~ 700 DEG C, 4 ~ 6h, heating rate
For 2 ~ 5 DEG C/min.
2. preparation method according to claim 1, which is characterized in that the nickel source is nickel nitrate or nickel acetate.
3. preparation method according to claim 1, which is characterized in that the titanium source is isopropyl titanate or the positive fourth of metatitanic acid
Ester.
4. preparation method according to claim 1, which is characterized in that the acid is nitric acid or acetic acid.
5. preparation method according to claim 1, which is characterized in that the drying temperature of low temperature drying described in step (1)
It is 40 ~ 60 DEG C, drying time is 6 ~ 20h.
6. the Ni-based nano particle catalysis material of multiphase metatitanic acid that any preparation method of claim 1 ~ 5 is prepared.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101168127A (en) * | 2007-11-28 | 2008-04-30 | 北京化工大学 | Nanometer semiconductor oxidation photocatalyst and preparation method thereof |
| US20100264097A1 (en) * | 2007-07-18 | 2010-10-21 | Nanyang Technological University | Hollow porous microspheres |
| CN102962068A (en) * | 2012-11-08 | 2013-03-13 | 浙江理工大学 | Nickel titanate catalyst for organic dyestuff degradation by visible light and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100264097A1 (en) * | 2007-07-18 | 2010-10-21 | Nanyang Technological University | Hollow porous microspheres |
| CN101168127A (en) * | 2007-11-28 | 2008-04-30 | 北京化工大学 | Nanometer semiconductor oxidation photocatalyst and preparation method thereof |
| CN102962068A (en) * | 2012-11-08 | 2013-03-13 | 浙江理工大学 | Nickel titanate catalyst for organic dyestuff degradation by visible light and preparation method thereof |
Non-Patent Citations (2)
| Title |
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| High-density NiTiO3/TiO2 nanotubes synthesized through sol-gel method using well-ordered TiO2 membranes as template;Dong Fang et al.;《Journal of Alloys and Compounds》;20100303;第498卷;第37-41页 |
| 介孔复合半导体NiO-TiO2的制备与光响应性能;王希涛 等;《无机材料学报》;20090331;第24卷(第2期);第215-220页 |
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