CN105905940B - A kind of preparation method of nickel titanate/titanium dioxide composite nano material - Google Patents
A kind of preparation method of nickel titanate/titanium dioxide composite nano material Download PDFInfo
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- CN105905940B CN105905940B CN201610222104.6A CN201610222104A CN105905940B CN 105905940 B CN105905940 B CN 105905940B CN 201610222104 A CN201610222104 A CN 201610222104A CN 105905940 B CN105905940 B CN 105905940B
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- titanium dioxide
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- nano material
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 34
- DGXKDBWJDQHNCI-UHFFFAOYSA-N dioxido(oxo)titanium nickel(2+) Chemical compound [Ni++].[O-][Ti]([O-])=O DGXKDBWJDQHNCI-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 33
- 239000002131 composite material Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- 238000004132 cross linking Methods 0.000 claims abstract description 23
- SHWZFQPXYGHRKT-FDGPNNRMSA-N (z)-4-hydroxypent-3-en-2-one;nickel Chemical compound [Ni].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O SHWZFQPXYGHRKT-FDGPNNRMSA-N 0.000 claims abstract description 16
- 230000001476 alcoholic effect Effects 0.000 claims abstract description 16
- 239000000203 mixture Substances 0.000 claims abstract description 15
- GYUPBLLGIHQRGT-UHFFFAOYSA-N pentane-2,4-dione;titanium Chemical compound [Ti].CC(=O)CC(C)=O GYUPBLLGIHQRGT-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000047 product Substances 0.000 claims description 31
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 15
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- 230000004044 response Effects 0.000 claims description 13
- 239000012467 final product Substances 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 3
- 238000006555 catalytic reaction Methods 0.000 abstract description 20
- 239000000463 material Substances 0.000 abstract description 16
- 238000007146 photocatalysis Methods 0.000 abstract description 15
- 230000001699 photocatalysis Effects 0.000 abstract description 15
- 230000015556 catabolic process Effects 0.000 abstract description 13
- 238000006731 degradation reaction Methods 0.000 abstract description 13
- 230000000694 effects Effects 0.000 abstract description 10
- 238000000034 method Methods 0.000 abstract description 10
- 239000012535 impurity Substances 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000010919 dye waste Substances 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000004659 sterilization and disinfection Methods 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 28
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 9
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 7
- 229940012189 methyl orange Drugs 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 6
- 238000005286 illumination Methods 0.000 description 6
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 6
- 229910052753 mercury Inorganic materials 0.000 description 6
- 239000011259 mixed solution Substances 0.000 description 6
- 239000001048 orange dye Substances 0.000 description 6
- 239000011941 photocatalyst Substances 0.000 description 6
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 6
- 238000001179 sorption measurement Methods 0.000 description 6
- 238000002798 spectrophotometry method Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 5
- 229910052759 nickel Inorganic materials 0.000 description 5
- 238000001816 cooling Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- -1 acyl acetone titanium Chemical compound 0.000 description 3
- 229910021543 Nickel dioxide Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- YDZQQRWRVYGNER-UHFFFAOYSA-N iron;titanium;trihydrate Chemical group O.O.O.[Ti].[Fe] YDZQQRWRVYGNER-UHFFFAOYSA-N 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- NICYNNGYHJJJMJ-UHFFFAOYSA-N propan-2-one;titanium Chemical compound [Ti].CC(C)=O NICYNNGYHJJJMJ-UHFFFAOYSA-N 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
-
- 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
-
- B01J35/39—
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention belongs to functional material preparing technical field, it is related to a kind of preparation method of nickel titanate/titanium dioxide composite nano material, by nickel acetylacetonate and titanium acetylacetone, after dissolving mix homogeneously in alcoholic solution, cross-linking reaction is carried out at a certain temperature, is then carried out heat treatment in Muffle furnace and is obtained nickel titanate/titanium dioxide composite nano material.Present invention process is simple and easy to do, and purity is high, and impurity content is low, and product preparation cost is low, excellent performance, can be with industrialized mass production.Nickel titanate/titanium dioxide composite nano material prepared by the present invention is used as catalysis material has higher catalysis activity, is with a wide range of applications in fields such as degradation of dye waste water and indoor harmful gas, photocatalysis disinfections.
Description
Technical field
The invention belongs to the preparing technical field of functional material, concretely relates to a kind of metatitanic acid nickel/titanium dioxide multiple
Close the preparation method of nano material.
Background technology
Nickel titanate (NiTiO3) belong to the trigonal system of ilmenite structure, it is widely used inorganic functional material, all
There is application in many industrial circles.Nickel titanate has high q-factor, low-k and good sound-optical and electrical-optical property, also has
There are semiconduction and weak magnetic, be widely used as semiconductor rectifier, the catalyst of bicarbonate and surface coated dyeing and mix
Mixture.In addition, nickel titanate can reduce friction and the cladding material being lost to be used as high temperature under conditions of not having fluid lubricant
Material.Additionally, nickel titanate is used as a kind of narrow band gap（2.18eV）Semi-conducting material, have good photoresponse in visible region,
There is tempting application prospect in terms of photocatalysis.Titanium dioxide is that stable chemical nature, catalysis activity are high, nontoxic, cheap
Catalysis material.But the energy gap of titanium dioxide (3.2 eV) is wider, relatively low for the utilization ratio of solar energy.Utilize
It is to improve one kind of conductor photocatalysis activity effectively that two kinds of catalysis materials are combined with each other and are prepared into the method for composite
Approach.Nickel titanate and titanium dioxide are combined with each other and prepare composite nano materials by the present invention.
It is traditional to prepare composite nano materials method, including solid sintering technology, coprecipitation, sol-gal process etc..These
Process needs complicated operation, and too high reaction temperature, long-time sintering process can make particle from caking, obtain product and do not fix
Pattern.Exploitation efficiently controls the pattern of nano material to be had to improving the performances such as optics, the catalysis of nano material with structure
Important effect.
The content of the invention
It is contemplated that it is low that a kind of preparation cost is provided in place of overcoming the deficiencies in the prior art, it is easy to operational control, mesh
Product yield high, homogeneity is good, and the preparation side of the nickel titanate/titanium dioxide composite nano material with higher catalytic activity
Method, realizes the technical process that composite nano materials powder body is produced in Low Temperature Solid-Phase calcining.By multigroup contrast test, crosslinking is found
Reaction plays an important role in preparation technology.Prepared nickel titanate/titanium dioxide composite nano material, with good light
Catalytic performance, under the process conditions of photocatalytic degradation of dye, degradation rate has reached more than 96% within 60 minutes.Preparation method of the present invention
The chemosynthesis research of other functional materials is can be applied equally to, and is had broad application prospects.
To reach above-mentioned purpose, what the present invention was realized in.
A kind of preparation method of nickel titanate/titanium dioxide composite nano material, its by nickel acetylacetonate and titanium acetylacetone,
After mix homogeneously being dissolved in alcoholic solution, carry out cross-linking reaction, after the pyroreaction that continues, temperature drop is to room at a certain temperature
Temperature, obtains final product purpose product.
As a kind of preferred version, nickel acetylacetonate of the present invention and titanium acetylacetone mol ratio be 1: 0.2～
5。
Further, nickel acetylacetonate of the present invention molar concentration in alcoholic solution is 0.01～1.0 mol/L.
Further, alcoholic solution of the present invention be methanol, one or two in ethanol, ethylene glycol, isopropanol
Mixture above.
Further, at 150～400 °C, cross-linking reaction time is 2～8 h to cross-linking reaction temperature of the present invention.
Further, at 600～1000 °C, the response time is 6～24 h to pyroreaction temperature of the present invention.
Compared with prior art, the present invention has following features.
（1）The present invention is developed and prepares nickel titanate/titanium dioxide composite nano material new technology route, and product cut size is 50
Between～100nm.The technique preparation cost is low, easy to control, with higher production efficiency, it is possible to achieve industrialization is big
Amount production.
（2）Purpose product yield（99.0%～99.6%）, product purity height（99.6%～99.8%）Industry can be met should
With requirement of the field to catalysis material product.
（3）Purpose product nickel titanate/titanium dioxide composite nano material prepared by the present invention is catalysis material, 60 minutes
Degradation rate can reach（99.5%～97.0%）, with higher catalysis activity.
Description of the drawings
The invention will be further described with reference to the accompanying drawings and detailed description.Protection scope of the present invention not only office
It is limited to the statement of following content.
Fig. 1 is the nickel titanate/titanium dioxide composite nano material SEM figures of the present invention.
Fig. 2 is the nickel titanate/titanium dioxide composite nano material SEM figures of the present invention.
Fig. 3 is the nickel titanate/titanium dioxide composite nano material SEM figures of the present invention.
Fig. 4 is the nickel titanate/titanium dioxide composite nano material X-ray diffractogram of the present invention.
Specific embodiment
The present invention designs a kind of chemical preparation process, prepares metatitanic acid nickel/titanium dioxide by new chemistry route and is combined
Nano material.Its photocatalysis property can be estimated by the typical methyl orange of photocatalytic degradation.
The present invention with nickel acetylacetonate and titanium acetylacetone, in alcoholic solution dissolve mix homogeneously after, at a certain temperature
Cross-linking reaction is carried out, after the pyroreaction that continues, temperature drop obtains final product purpose product to room temperature.
Preparation process of the present invention is.
（1）By nickel acetylacetonate and titanium acetylacetone, mix homogeneously, nickel acetylacetonate and levulinic are dissolved in alcoholic solution
The mol ratio of ketone titanium is 1: 0.2～5；Nickel acetylacetonate molar concentration in alcoholic solution is 0.02～1.0 mol/L；Alcoholic solution is
For one or more the mixture in methanol, ethanol, ethylene glycol, isopropanol.
（2）By the mixed solution for obtaining at a certain temperature, cross-linking reaction is carried out, cross-linking reaction temperature is at 150～400 °
C, cross-linking reaction time are 2～8 h.
（3）Cross-linking reaction terminates, then carries out high-temperature calcination, and at 600～1000 °C, the response time is 6 to pyroreaction temperature
～24 h, temperature drop obtain final product purpose product to room temperature.
（4）By the use of prepared nickel titanate/titanium dioxide composite nano material as photocatalyst（0.2g/L）, degraded
The methyl orange solution of 20mg/L.In photocatalysis experiment, light source used is 500W mercury lamps.Before irradiation, the methyl containing catalysis material
Orange solution is stirred 30 minutes in the dark, carries out illumination after reaching adsorption equilibrium.It is dense with spectrophotometric determination methyl orange dye
Degree change.
Referring to the nickel titanate/titanium dioxide composite nano material SEM figures for shown in Fig. 1～3, being the present invention, it can be seen that produce
Thing is the preferable nanoparticle of homogeneity.Fig. 4 is the nickel titanate/titanium dioxide composite nano material X-ray diffractogram of the present invention,
Diffraction maximums of the wherein # for nickel titanate, diffraction maximums of the * for titanium dioxide.
Embodiment 1.
The aqueous isopropanol that concentration is 0.2 mol/L nickel acetylacetonates is slowly dropped to into the second that concentration is 0.2 mol/L
In the aqueous isopropanol of acyl acetone titanium, mix homogeneously is dissolved in alcoholic solution.The mixed solution for obtaining is carried out into cross-linking reaction, instead
Answer temperature at 200 °C, the response time is 4 hours, and wherein the mol ratio of nickel acetylacetonate and titanium acetylacetone is 1: 2.Crosslinking is anti-
After should terminating, pyroreaction in being connected at Muffle furnace, is carried out, at 600 °C, the response time is 24 h to pyroreaction temperature.It is natural
After cooling, that is, obtain purpose product.
Between 50～70nm, the yield of product is 99.6% to product cut size.Product purity is 99.8%, impurity content：Carbon
Less than 0.2%.By the use of prepared nickel titanate/titanium dioxide composite nano material as photocatalyst（0.2g/L）, degraded
The methyl orange solution of 20mg/L.In photocatalysis experiment, light source used is 500W mercury lamps.Before irradiation, the methyl containing catalysis material
Orange solution is stirred 30 minutes in the dark, carries out illumination after reaching adsorption equilibrium.It is dense with spectrophotometric determination methyl orange dye
Degree, calculates degradation rate.In the test that catalysis activity is evaluated in photocatalysis, the degradation rate of 60 minutes is 99.5%.
Embodiment 2.
The methanol solution that concentration is 0.2 mol/L nickel acetylacetonates is slowly dropped to into the acetyl that concentration is 0.2 mol/L
The methanol solution of acetone titanium, dissolves mix homogeneously in alcoholic solution.The mixed solution for obtaining is carried out into cross-linking reaction, reaction temperature
At 300 °C, the response time is 8 hours, and wherein the mol ratio of nickel acetylacetonate and titanium acetylacetone is 1: 2.Cross-linking reaction terminates
Afterwards, pyroreaction is carried out in being connected at Muffle furnace, at 1000 °C, the response time is 6 h to pyroreaction temperature.After natural cooling,
Purpose product is obtained.
Between 60～80nm, the yield of product is 99.2% to product cut size.Product purity is not less than 99.7%, and impurity contains
Amount：Carbon is less than 0.3%.By the use of prepared nickel titanate/titanium dioxide composite nano material as photocatalyst（0.2g/L）, drop
The methyl orange solution of solution 20mg/L.In photocatalysis experiment, light source used is 500W mercury lamps.Before irradiation, the first containing catalysis material
Base orange solution is stirred 30 minutes in the dark, carries out illumination after reaching adsorption equilibrium.Use spectrophotometric determination methyl orange dye
Concentration, calculates degradation rate.In the test that catalysis activity is evaluated in photocatalysis, the degradation rate of 60 minutes is 98.5%.
Embodiment 3.
The ethanol solution that concentration is 0.02 mol/L nickel acetylacetonates is slowly dropped to into the second that concentration is 0.02 mol/L
The ethanol solution of acyl acetone titanium, dissolves mix homogeneously in alcoholic solution.The mixed solution for obtaining is carried out into cross-linking reaction, reaction temperature
At 150 °C, the response time is 8 hours to degree, and wherein the mol ratio of nickel acetylacetonate and titanium acetylacetone is 1: 2.Cross-linking reaction is tied
Shu Hou, carries out pyroreaction in being connected at Muffle furnace, at 1000 °C, the response time is 6 h to pyroreaction temperature.Natural cooling
Afterwards, that is, obtain purpose product.
Between 60～70nm, the yield of product is 99.5% to product cut size.Product purity is not less than 99.6%, and impurity contains
Amount：Carbon is less than 0.4%.By the use of prepared nickel titanate/titanium dioxide composite nano material as photocatalyst（0.2g/L）, drop
The methyl orange solution of solution 20mg/L.In photocatalysis experiment, light source used is 500W mercury lamps.Before irradiation, the first containing catalysis material
Base orange solution is stirred 30 minutes in the dark, carries out illumination after reaching adsorption equilibrium.Use spectrophotometric determination methyl orange dye
Concentration, calculates degradation rate.In the test that catalysis activity is evaluated in photocatalysis, the degradation rate of 60 minutes is 97.8%.
Embodiment 4.
The aqueous isopropanol that concentration is 0.1 mol/L nickel acetylacetonates is slowly dropped to into the second that concentration is 0.1 mol/L
The aqueous isopropanol of acyl acetone titanium, dissolves mix homogeneously in alcoholic solution.The mixed solution for obtaining is carried out into cross-linking reaction, is reacted
At 400 °C, the response time is 4 hours to temperature, and wherein the mol ratio of nickel acetylacetonate and titanium acetylacetone is 1: 2.Cross-linking reaction
After end, pyroreaction in being connected at Muffle furnace, is carried out, at 800 °C, the response time is 10 h to pyroreaction temperature.Naturally it is cold
But after, that is, obtain purpose product.
Between 80～100nm, the yield of product is 99.5% to product cut size.Product purity is not less than 99.7%, and impurity contains
Amount：Carbon is less than 0.3%.By the use of prepared nickel titanate/titanium dioxide composite nano material as photocatalyst（0.2g/L）, drop
The methyl orange solution of solution 20mg/L.In photocatalysis experiment, light source used is 500W mercury lamps.Before irradiation, the first containing catalysis material
Base orange solution is stirred 30 minutes in the dark, carries out illumination after reaching adsorption equilibrium.Use spectrophotometric determination methyl orange dye
Concentration, calculates degradation rate.In the test that catalysis activity is evaluated in photocatalysis, the degradation rate of 60 minutes is 99.4%.
Embodiment 5.
It is 0.02 mol/L that the ethylene glycol solution that concentration is 0.02 mol/L nickel acetylacetonates is slowly dropped to concentration
In the ethylene glycol solution of titanium acetylacetone, mix homogeneously is dissolved in alcoholic solution.The mixed solution for obtaining is carried out into cross-linking reaction,
At 300 °C, the response time is 8 hours to reaction temperature, and wherein the mol ratio of nickel acetylacetonate and titanium acetylacetone is 1: 2.Crosslinking
After reaction terminates, pyroreaction in being connected at Muffle furnace, is carried out, at 1000 °C, the response time is 12 h to pyroreaction temperature.From
After so cooling down, that is, obtain purpose product.
Between 60～100nm, the yield of product is 99.5% to product cut size.Product purity is not less than 99.6%, and impurity contains
Amount：Carbon is less than 0.4%.By the use of prepared nickel titanate/titanium dioxide composite nano material as photocatalyst（0.2g/L）, drop
The methyl orange solution of solution 20mg/L.In photocatalysis experiment, light source used is 500W mercury lamps.Before irradiation, the first containing catalysis material
Base orange solution is stirred 30 minutes in the dark, carries out illumination after reaching adsorption equilibrium.Use spectrophotometric determination methyl orange dye
Concentration, calculates degradation rate.In the test that catalysis activity is evaluated in photocatalysis, the degradation rate of 60 minutes is 97.0%.
The preferred embodiments of the present invention are the foregoing is only, the present invention is not limited to, for the skill of this area
For art personnel, the present invention can have various modifications and variations.It is all within the spirit and principles in the present invention, made any repair
Change, equivalent, improvement etc., should be included within the scope of the present invention.
Claims (5)
1. a kind of preparation method of nickel titanate/titanium dioxide composite nano material, it is characterised in that by nickel acetylacetonate and acetyl
Acetone titanium, after dissolving mix homogeneously, carries out cross-linking reaction, after the pyroreaction that continues, temperature in alcoholic solution at a certain temperature
Room temperature is dropped to, purpose product is obtained final product；The mol ratio of described nickel acetylacetonate and titanium acetylacetone is 1: 2.
2. the preparation method of nickel titanate/titanium dioxide composite nano material according to claim 1, it is characterised in that：Institute
The nickel acetylacetonate stated molar concentration in alcoholic solution is 0.02～1.0 mol/L.
3. the preparation method of nickel titanate/titanium dioxide composite nano material according to claim 2, it is characterised in that：Institute
The alcoholic solution stated is methanol, one or more the mixture in ethanol, ethylene glycol, isopropanol.
4. the preparation method of nickel titanate/titanium dioxide composite nano material according to claim 3, it is characterised in that：Institute
At 150～400 DEG C, cross-linking reaction time is 2～8 h to the cross-linking reaction temperature stated.
5. the preparation method of nickel titanate/titanium dioxide composite nano material according to claim 4, it is characterised in that：Institute
At 600～1000 DEG C, the response time is 6～24 h to the pyroreaction temperature stated.
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| CN106241853B (en) * | 2016-09-12 | 2018-02-27 | 渤海大学 | A kind of preparation method of yittrium oxide nano material |
| CN106348342B (en) * | 2016-09-12 | 2018-03-20 | 渤海大学 | A kind of preparation method of spherical zirconic acid lanthanum nano material |
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