CN110280248A - A kind of preparation method of nickel titanate/titanic oxide nano compound material - Google Patents
A kind of preparation method of nickel titanate/titanic oxide nano compound material Download PDFInfo
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- CN110280248A CN110280248A CN201910652044.5A CN201910652044A CN110280248A CN 110280248 A CN110280248 A CN 110280248A CN 201910652044 A CN201910652044 A CN 201910652044A CN 110280248 A CN110280248 A CN 110280248A
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title claims abstract description 44
- 239000000463 material Substances 0.000 title claims abstract description 22
- 150000001875 compounds Chemical class 0.000 title claims abstract description 17
- DGXKDBWJDQHNCI-UHFFFAOYSA-N dioxido(oxo)titanium nickel(2+) Chemical compound [Ni++].[O-][Ti]([O-])=O DGXKDBWJDQHNCI-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 239000013099 nickel-based metal-organic framework Substances 0.000 claims abstract description 33
- 239000002114 nanocomposite Substances 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 13
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 44
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 39
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 34
- 238000001035 drying Methods 0.000 claims description 32
- 238000003756 stirring Methods 0.000 claims description 31
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 30
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 30
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 27
- 238000006243 chemical reaction Methods 0.000 claims description 25
- 238000005406 washing Methods 0.000 claims description 24
- 239000008367 deionised water Substances 0.000 claims description 18
- 229910021641 deionized water Inorganic materials 0.000 claims description 18
- 239000007864 aqueous solution Substances 0.000 claims description 16
- 238000001354 calcination Methods 0.000 claims description 15
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 13
- 239000000843 powder Substances 0.000 claims description 12
- 238000005119 centrifugation Methods 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 229960004756 ethanol Drugs 0.000 claims 1
- 235000019441 ethanol Nutrition 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 12
- 238000007146 photocatalysis Methods 0.000 abstract description 10
- 230000015556 catabolic process Effects 0.000 abstract description 3
- 238000000354 decomposition reaction Methods 0.000 abstract description 3
- 238000006731 degradation reaction Methods 0.000 abstract description 3
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 3
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 3
- 239000002131 composite material Substances 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 22
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 8
- 229960000907 methylthioninium chloride Drugs 0.000 description 8
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000002604 ultrasonography Methods 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 239000012621 metal-organic framework Substances 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000004449 solid propellant Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
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- 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
- 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
-
- 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
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
-
- 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
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/51—Spheres
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
Abstract
A kind of preparation method of nickel titanate/titanic oxide nano compound material, is related to a kind of TiO2The preparation method of nanocomposite.The present invention is to solve TiO2Under visible light without photocatalysis performance the problem of.The present invention: one, presoma Ni-MOF is prepared；Two, NiTiO3/TiO2The preparation of nanocomposite.The present invention prepares presoma Ni-MOF using hydro-thermal method, and simple process combines NiTiO3And TiO2Two kinds of respective characteristic and advantages of material, in organic pollutant degradation, water decomposition and CO2The photocatalysis fields such as reduction have great application prospect.The present invention is by by TiO2And NiTiO3It is compound, widen TiO2Photoresponse region, so that composite material can play preferable photocatalysis under sunlight, Ni-MOF spherical structure is complete, and size is about 600nm.
Description
Technical field
The present invention relates to a kind of TiO2The preparation method of nanocomposite.
Background technique
With the increasingly reduction of fossil fuel reserves, luminous energy has wide as a kind of inexhaustible, nexhaustible energy
Wealthy application prospect, there is consequence in modern development.Luminous energy be converted to electric energy or chemical energy be always one very
Important research direction.
Semiconductor material TiO2The catalytic activity of Yin Qigao, good chemical stability, cheap price and nontoxic
The advantages that be widely used in organic pollutant degradation, water decomposition and CO2The fields such as reduction.But for photocatalysis performance, TiO2
Forbidden band is wider, is only capable of absorbing the ultraviolet light in sunlight, thus photocatalysis performance is restricted.In recent years, by TiO2With forbidden band
The lesser Material cladding of width improves photocatalytic activity, it has also become TiO to widen its photoresponse region2The heat of photocatalysis field
Point.
For a long time, ternary oxide has ten in fields such as solid fuel cell, sensor, chemical catalysis and photocatalysis
Divide and is widely applied.As the Typical Representative of ternary oxide, due to NiTiO3(nickel titanate) has catalytic activity height, stability
Well, the advantages that durability is good under ultraviolet light and can respond under visible light receives in photocatalytic applications wide
General concern.
Summary of the invention
The present invention is to solve TiO2Under visible light without photocatalysis performance the technical issues of, and provide a kind of applied to light
Nickel titanate/titanic oxide nano compound material preparation method of catalysis.
Preparation method applied to light-catalysed nickel titanate/titanic oxide nano compound material of the invention is by following step
Suddenly it carries out:
One, presoma Ni-MOF is prepared: by Ni (NO3)2·6H2O and terephthalic acid (TPA) are added in dimethylformamide,
Stirring is completely dissolved to solid, is added ethylene glycol and is continued to stir 20min~30min, mixed liquor I is obtained, then by mixed liquor I
It moves into reaction kettle, reaction kettle is placed in baking oven heats 6h~12h under conditions of temperature is 120 DEG C~130 DEG C, finally successively
Through centrifugation, washing and drying, presoma Ni-MOF is obtained；
Ni (NO in the mixed liquor I3)2·6H2The molar concentration of O is 0.018mol/L~0.022mol/L；
The molar concentration of terephthalic acid (TPA) is 0.007mol/L~0.012mol/L in the mixed liquor I；
The volume ratio of the ethylene glycol and dimethylformamide is (0.12~0.35): 1；
Washing described in step 1 is successively to be washed using DMF and dehydrated alcohol；
Two, NiTiO3/TiO2The preparation of nanocomposite: by step 1 preparation presoma Ni-MOF ultrasonic disperse in
5min~10min in dehydrated alcohol stirs 10min~15min, tetra-n-butyl titanate is added dropwise under stirring conditions, so
10min~20min is stirred afterwards, obtains mixed liquor II, then deionized water and hydrofluoric acid aqueous solution are added into mixed liquor II, stirring
10min~15min is subsequently moved in reaction kettle, and reaction kettle is placed in baking oven under conditions of temperature is 180 DEG C~200 DEG C
8h~20h is heated, then successively obtains shallow green powder through centrifugation, washing and drying；In air atmosphere by shallow green powder
It is calcined in Muffle furnace, calcination temperature is 550 DEG C~650 DEG C, and calcination time is 2h~5h, and heating rate is 2 DEG C/min~8
DEG C/min, obtain NiTiO3/TiO2Nanocomposite；
The mass concentration of the hydrofluoric acid aqueous solution is 40%；
The concentration of tetra-n-butyl titanate is 0.01mol/L~0.016mol/L in the mixed liquor II；
The volume ratio of the deionized water and dehydrated alcohol is (0.05~0.08): 1；
The volume ratio of the hydrofluoric acid aqueous solution and dehydrated alcohol is (0.00075~0.002): 1；
The concentration for the presoma Ni-MOF that in the mixed liquor II prepared by step 1 is 0.5g/L~0.75g/L；
Washing described in step 2 is successively to be washed using deionized water and dehydrated alcohol.
Existing preparation method is mostly with TiO2For core, in TiO2Surrounding cladding NiO prepares NiTiO3/TiO2；And it is of the invention
Preparation method provides nickel source by predecessor of MOF, is converted into NiTiO in hydro-thermal reaction and high-temperature burning process3/TiO2。
Beneficial effects of the present invention:
1, the present invention prepares presoma Ni-MOF, simple process using hydro-thermal method；
2, the novel NiTiO that preparation method of the invention obtains3/TiO2Nanocomposite combines NiTiO3And TiO2
Two kinds of respective characteristic and advantages of material, in organic pollutant degradation, water decomposition and CO2The photocatalysis fields such as reduction have very
Big application prospect.
3, the present invention is by by TiO2And NiTiO3It is compound, widen TiO2Photoresponse region, so that composite material is in sunlight
Under can play preferable photocatalysis；
4, Ni-MOF spherical structure prepared by the present invention is complete, and size is about 600nm.
Detailed description of the invention
Fig. 1 is XRD diagram；
Fig. 2 is the SEM figure of the presoma Ni-MOF high power of one preparation the step of testing one；
Fig. 3 is the SEM figure of the presoma Ni-MOF low power of one preparation the step of testing one；
Fig. 4 is the NiTiO of two preparations the step of testing one3/TiO2First SEM of nanocomposite schemes；
Fig. 5 is the NiTiO of two preparations the step of testing one3/TiO22nd SEM of nanocomposite schemes；
Fig. 6 is the curve graph for testing photocatalytic degradation methylene blue in four.
Specific embodiment
Specific embodiment 1: present embodiment is a kind of applied to light-catalysed NiTiO3/TiO2Nanocomposite
Preparation method specifically carries out according to the following steps:
One, presoma Ni-MOF is prepared: by Ni (NO3)2·6H2O and terephthalic acid (TPA) are added in dimethylformamide,
Stirring is completely dissolved to solid, is added ethylene glycol and is continued to stir 20min~30min, mixed liquor I is obtained, then by mixed liquor I
It moves into reaction kettle, reaction kettle is placed in baking oven heats 6h~12h under conditions of temperature is 120 DEG C~130 DEG C, finally successively
Through centrifugation, washing and drying, presoma Ni-MOF is obtained；
Ni (NO in the mixed liquor I3)2·6H2The molar concentration of O is 0.018mol/L~0.022mol/L；
The molar concentration of terephthalic acid (TPA) is 0.007mol/L~0.012mol/L in the mixed liquor I；
The volume ratio of the ethylene glycol and dimethylformamide is (0.12~0.35): 1；
Washing described in step 1 is successively to be washed using DMF and dehydrated alcohol；
Two, NiTiO3/TiO2The preparation of nanocomposite: by step 1 preparation presoma Ni-MOF ultrasonic disperse in
5min~10min in dehydrated alcohol stirs 10min~15min, tetra-n-butyl titanate is added dropwise under stirring conditions, so
10min~20min is stirred afterwards, obtains mixed liquor II, then deionized water and hydrofluoric acid aqueous solution are added into mixed liquor II, stirring
10min~15min is subsequently moved in reaction kettle, and reaction kettle is placed in baking oven under conditions of temperature is 180 DEG C~200 DEG C
8h~20h is heated, then successively obtains shallow green powder through centrifugation, washing and drying；In air atmosphere by shallow green powder
It is calcined in Muffle furnace, calcination temperature is 550 DEG C~650 DEG C, and calcination time is 2h~5h, and heating rate is 2 DEG C/min~8
DEG C/min, obtain NiTiO3/TiO2Nanocomposite；
The mass concentration of the hydrofluoric acid aqueous solution is 40%；
The concentration of tetra-n-butyl titanate is 0.01mol/L~0.016mol/L in the mixed liquor II；
The volume ratio of the deionized water and dehydrated alcohol is (0.05~0.08): 1；
The volume ratio of the hydrofluoric acid aqueous solution and dehydrated alcohol is (0.00075~0.002): 1；
The concentration for the presoma Ni-MOF that in the mixed liquor II prepared by step 1 is 0.5g/L~0.75g/L；
Washing described in step 2 is successively to be washed using deionized water and dehydrated alcohol.
Specific embodiment 2: the present embodiment is different from the first embodiment in that: drying described in step 1
Temperature be 60 DEG C, drying time 10h.Other are same as the specific embodiment one.
Specific embodiment 3: the present embodiment is different from the first and the second embodiment in that: it is described in step 1
The molar concentration of terephthalic acid (TPA) is 0.01mol/L in mixed liquor I.Other are the same as one or two specific embodiments.
Specific embodiment 4: unlike one of present embodiment and specific embodiment one to three: institute in step 1
Ni (NO in the mixed liquor I stated3)2·6H2The molar concentration of O is 0.02mol/L.One of other and specific embodiment one to three
It is identical.
Specific embodiment 5: present embodiment is unlike specific embodiment four: second two described in step 1
The volume ratio of alcohol and dimethylformamide is 0.2:1.Other are identical as specific embodiment four.
Specific embodiment 6: unlike one of present embodiment and specific embodiment one to five: institute in step 2
The temperature for the drying stated is 60 DEG C, and drying time is for 24 hours.Other are identical as one of specific embodiment one to five.
Specific embodiment 7: unlike one of present embodiment and specific embodiment one to six: institute in step 2
The concentration of tetra-n-butyl titanate is 0.012mol/L in the mixed liquor II stated.One of other and specific embodiment one to six phase
Together.
Specific embodiment 8: unlike one of present embodiment and specific embodiment one to seven: institute in step 2
The volume ratio of the deionized water and dehydrated alcohol stated is 0.07:1.Other are identical as one of specific embodiment one to seven.
Specific embodiment 9: unlike one of present embodiment and specific embodiment one to eight: institute in step 2
The volume ratio of the hydrofluoric acid and dehydrated alcohol stated is 0.001:1.Other are identical as one of specific embodiment one to eight.
The present invention is verified with following tests:
Test one: this test is a kind of applied to light-catalysed NiTiO3/TiO2The preparation method of nanocomposite, tool
Body carries out according to the following steps:
One, presoma Ni-MOF is prepared: by the Ni (NO of 0.21g3)2·6H2O and 0.05g terephthalic acid (TPA) is added to 40mL
Dimethylformamide in, stirring 20min be completely dissolved to solid, add 5mL ethylene glycol continue stir 20min, mixed
Liquid I is closed, then moves into mixed liquor I in reaction kettle, reaction kettle, which is placed in baking oven, heats 6h under conditions of temperature is 120 DEG C,
Finally successively through centrifugation, washing and drying, presoma Ni-MOF is obtained；
Washing described in step 1 is successively to be washed using DMF and dehydrated alcohol；
The temperature of drying described in step 1 is 60 DEG C, drying time 10h；
Two, NiTiO3/TiO2The preparation of nanocomposite: presoma Ni-MOF ultrasound prepared by 0.03g step 1 point
The 5min in the dehydrated alcohol of 40mL is dissipated, 10min is stirred, the tetra-n-butyl titanate of 150 μ l is added dropwise under stirring conditions,
Then stir 10min, obtain mixed liquor II, then into mixed liquor II be added 2.8mL deionized water and 30 μ l hydrofluoric acid water
Solution stirs 10min, is subsequently moved in reaction kettle, and reaction kettle is placed in baking oven and is heated under conditions of temperature is 180 DEG C
Then 8h successively obtains shallow green powder through centrifugation, washing and drying；By shallow green powder in air atmosphere in Muffle furnace
Middle calcining, calcination temperature are 550 DEG C, calcination time 2h, and heating rate is 2 DEG C/min, obtain NiTiO3/TiO2It is nano combined
Material；
The mass concentration of the hydrofluoric acid aqueous solution is 40%；
Washing described in step 2 is successively to be washed using deionized water and dehydrated alcohol；
The temperature of drying described in step 2 is 60 DEG C, and drying time is for 24 hours.
Test two: this test is a kind of applied to light-catalysed NiTiO3/TiO2The preparation method of nanocomposite, tool
Body carries out according to the following steps:
One, presoma Ni-MOF is prepared: by the Ni (NO of 0.23g3)2·6H2O and 0.06g terephthalic acid (TPA) is added to 40mL
Dimethylformamide in, stirring 30min be completely dissolved to solid, add 10mL ethylene glycol continue stir 20min, mixed
Liquid I is closed, then moves into mixed liquor I in reaction kettle, reaction kettle, which is placed in baking oven, heats 6h under conditions of temperature is 120 DEG C,
Finally successively through centrifugation, washing and drying, presoma Ni-MOF is obtained；
Washing described in step 1 is successively to be washed using DMF and dehydrated alcohol；
The temperature of drying described in step 1 is 60 DEG C, drying time 10h；
Two, NiTiO3/TiO2The preparation of nanocomposite: the presoma Ni-MOF ultrasound that the step of 0.03g one is prepared
It is scattered in 5min in the dehydrated alcohol of 40mL, 10min is stirred, the positive fourth of metatitanic acid four of 200 μ l is added dropwise under stirring conditions
Then ester stirs 10min, obtain mixed liquor II, then into mixed liquor II be added 3mL deionized water and 30 μ l hydrofluoric acid water
Solution stirs 10min, is subsequently moved in reaction kettle, and reaction kettle is placed in baking oven and is heated under conditions of temperature is 180 DEG C
Then 8h successively obtains shallow green powder through centrifugation, washing and drying；By shallow green powder in air atmosphere in Muffle furnace
Middle calcining, calcination temperature are 600 DEG C, calcination time 4h, and heating rate is 5 DEG C/min, obtain NiTiO3/TiO2It is nano combined
Material；
The mass concentration of the hydrofluoric acid aqueous solution is 40%；
Washing described in step 2 is successively to be washed using deionized water and dehydrated alcohol；
The temperature of drying described in step 2 is 60 DEG C, and drying time is for 24 hours.
Test three: this test is a kind of applied to light-catalysed NiTiO3/TiO2The preparation method of nanocomposite, tool
Body carries out according to the following steps:
One, presoma Ni-MOF is prepared: by the Ni (NO of 0.25g3)2·6H2O and 0.07g terephthalic acid (TPA) is added to 40mL
Dimethylformamide in, stirring 20min be completely dissolved to solid, add 10mL ethylene glycol continue stir 20min, mixed
Liquid I is closed, then moves into mixed liquor I in reaction kettle, reaction kettle, which is placed in baking oven, heats 10h under conditions of temperature is 120 DEG C,
Finally successively through centrifugation, washing and drying, presoma Ni-MOF is obtained；
Washing described in step 1 is successively to be washed using DMF and dehydrated alcohol；
The temperature of drying described in step 1 is 60 DEG C, drying time 10h；
Two, NiTiO3/TiO2The preparation of nanocomposite: the presoma Ni-MOF ultrasound that the step of 0.02g one is prepared
It is scattered in 5min in the dehydrated alcohol of 40mL, 10min is stirred, the positive fourth of metatitanic acid four of 200 μ l is added dropwise under stirring conditions
Then ester stirs 10min, obtain mixed liquor II, then into mixed liquor II be added 2.8mL deionized water and 80 μ l hydrofluoric acid
Aqueous solution stirs 10min, is subsequently moved in reaction kettle, and reaction kettle is placed in baking oven and is heated under conditions of temperature is 180 DEG C
Then 10h successively obtains shallow green powder through centrifugation, washing and drying；By shallow green powder in air atmosphere in Muffle furnace
Middle calcining, calcination temperature are 550 DEG C, calcination time 2h, and heating rate is 2 DEG C/min, obtain NiTiO3/TiO2It is nano combined
Material；
The mass concentration of the hydrofluoric acid aqueous solution is 40%；
Washing described in step 2 is successively to be washed using deionized water and dehydrated alcohol；
The temperature of drying described in step 2 is 60 DEG C, and drying time is for 24 hours.
Fig. 1 is XRD diagram, ◆ it is TiO2, ★ NiTiO3, curve a is the presoma Ni- of one preparation the step of testing one
MOF, curve b are the TiO of standard2Curve, curve c are the NiTiO of two preparations the step of testing one3/TiO2Nanocomposite,
It can be seen that method of the invention successfully prepares Ni-MOF and NiTiO3/TiO2.In NiTiO3/TiO2XRD diagram in do not send out
The diffraction maximum of existing predecessor Ni-MOF and NiO, illustrate that it is transformed into NiTiO completely3/TiO2In.
The step of Fig. 2 is the SEM figure of the presoma Ni-MOF high power of one preparation the step of testing one, and Fig. 3 is test one one
The SEM of the presoma Ni-MOF low power of preparation schemes, and as can be seen from the figure Ni-MOF spherical structure is complete, and size is about 600nm.
Fig. 4 is the NiTiO of two preparations the step of testing one3/TiO2First SEM of nanocomposite schemes, and Fig. 5 is test
NiTiO prepared by one the step of two3/TiO22nd SEM of nanocomposite schemes, and as can be seen from the figure moiety complex is protected
The spherical morphology of presoma is held.
Test four: configuration concentration is the aqueous solution of methylene blue of 30ppm, takes the aqueous solution of methylene blue and 50mL of 50mL
Deionized water is mixed, the static 2h under no light condition, and the mass fraction that 250 μ L are then added into mixed liquor is 30%
H2O2The NiTiO of one preparation of aqueous solution and 20mg test3/TiO2Then nanocomposite carries out illumination drop under visible light
Solution remembers that the concentration of methylene blue at this time is initial concentration C0；
Every 20min takes 4mL sample, using ultraviolet specrophotometer carry out absorbance test, and according to standard curve into
The conversion of row concentration.Finally relative concentration is changed with time and is mapped.
Fig. 6 is the curve graph for testing photocatalytic degradation methylene blue in four, and ordinate is relative concentration=Ct/C0, Ct is
Concentration of the methylene blue in t moment, C0For the initial concentration of methylene blue, NiTiO as seen from the figure3/TiO2Nanocomposite tool
There is preferable catalytic effect, methylene blue is completely degraded after 107min.
Claims (9)
1. a kind of preparation method applied to light-catalysed nickel titanate/titanic oxide nano compound material, it is characterised in that application
It is carried out according to the following steps in the preparation method of light-catalysed nickel titanate/titanic oxide nano compound material:
One, presoma Ni-MOF is prepared: by Ni (NO3)2·6H2O and terephthalic acid (TPA) are added in dimethylformamide, stirring
It is completely dissolved to solid, adds ethylene glycol and continue to stir 20min~30min, obtain mixed liquor I, then move into mixed liquor I
In reaction kettle, reaction kettle be placed in baking oven temperature be 120 DEG C~130 DEG C under conditions of heat 6h~12h, finally successively through from
The heart, washing and drying obtain presoma Ni-MOF；
Ni (NO in the mixed liquor I3)2·6H2The molar concentration of O is 0.018mol/L~0.022mol/L；
The molar concentration of terephthalic acid (TPA) is 0.007mol/L~0.012mol/L in the mixed liquor I；
The volume ratio of the ethylene glycol and dimethylformamide is (0.12~0.35): 1；
Washing described in step 1 is successively to be washed using DMF and dehydrated alcohol；
Two, NiTiO3/TiO2The preparation of nanocomposite: by the presoma Ni-MOF ultrasonic disperse of step 1 preparation in anhydrous
5min~10min in ethyl alcohol stirs 10min~15min, tetra-n-butyl titanate is added dropwise under stirring conditions, then stirs
10min~20min is mixed, mixed liquor II is obtained, then deionized water and hydrofluoric acid aqueous solution are added into mixed liquor II, stirring
10min~15min is subsequently moved in reaction kettle, and reaction kettle is placed in baking oven under conditions of temperature is 180 DEG C~200 DEG C
8h~20h is heated, then successively obtains shallow green powder through centrifugation, washing and drying；In air atmosphere by shallow green powder
It is calcined in Muffle furnace, calcination temperature is 550 DEG C~650 DEG C, and calcination time is 2h~5h, and heating rate is 2 DEG C/min~8
DEG C/min, obtain NiTiO3/TiO2Nanocomposite；
The mass concentration of the hydrofluoric acid aqueous solution is 40%；
The molar concentration of tetra-n-butyl titanate is 0.01mol/L~0.016mol/L in the mixed liquor II；
The volume ratio of the deionized water and dehydrated alcohol is (0.05~0.08): 1；
The volume ratio of the hydrofluoric acid aqueous solution and dehydrated alcohol is (0.00075~0.002): 1；
The concentration for the presoma Ni-MOF that in the mixed liquor II prepared by step 1 is 0.5g/L~0.75g/L；
Washing described in step 2 is successively to be washed using deionized water and dehydrated alcohol.
2. a kind of preparation applied to light-catalysed nickel titanate/titanic oxide nano compound material according to claim 1
Method, it is characterised in that the temperature of drying described in step 1 is 60 DEG C, drying time 10h.
3. a kind of preparation applied to light-catalysed nickel titanate/titanic oxide nano compound material according to claim 1
Method, it is characterised in that the molar concentration of terephthalic acid (TPA) is 0.01mol/L in mixed liquor I described in step 1.
4. a kind of preparation applied to light-catalysed nickel titanate/titanic oxide nano compound material according to claim 1
Method, it is characterised in that Ni (NO in mixed liquor I described in step 13)2·6H2The molar concentration of O is 0.02mol/L.
5. a kind of preparation applied to light-catalysed nickel titanate/titanic oxide nano compound material according to claim 1
Method, it is characterised in that the volume ratio of ethylene glycol and dimethylformamide described in step 1 is 0.2:1.
6. a kind of preparation applied to light-catalysed nickel titanate/titanic oxide nano compound material according to claim 1
Method, it is characterised in that the temperature of drying described in step 2 is 60 DEG C, and drying time is for 24 hours.
7. a kind of preparation applied to light-catalysed nickel titanate/titanic oxide nano compound material according to claim 1
Method, it is characterised in that the concentration of tetra-n-butyl titanate is 0.012mol/L in mixed liquor II described in step 2.
8. a kind of preparation applied to light-catalysed nickel titanate/titanic oxide nano compound material according to claim 1
Method, it is characterised in that deionized water described in step 2 and the volume ratio of dehydrated alcohol are 0.07:1.
9. a kind of preparation applied to light-catalysed nickel titanate/titanic oxide nano compound material according to claim 1
Method, it is characterised in that the volume ratio of hydrofluoric acid described in step 2 and dehydrated alcohol is 0.001:1.
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| CN114832825B (en) * | 2022-05-18 | 2024-02-09 | 东南大学 | Preparation method of spherical shell separation double-coating structure catalyst |
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