CN105905940A - Preparation method of nickel titanate/titanium dioxide composite nanomaterial - Google Patents
Preparation method of nickel titanate/titanium dioxide composite nanomaterial Download PDFInfo
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- CN105905940A CN105905940A CN201610222104.6A CN201610222104A CN105905940A CN 105905940 A CN105905940 A CN 105905940A CN 201610222104 A CN201610222104 A CN 201610222104A CN 105905940 A CN105905940 A CN 105905940A
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- titanium dioxide
- dioxide composite
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- nickel titanate
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 70
- DGXKDBWJDQHNCI-UHFFFAOYSA-N dioxido(oxo)titanium nickel(2+) Chemical compound [Ni++].[O-][Ti]([O-])=O DGXKDBWJDQHNCI-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 36
- 239000002131 composite material Substances 0.000 title claims abstract description 35
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 26
- 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 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- GYUPBLLGIHQRGT-UHFFFAOYSA-N pentane-2,4-dione;titanium Chemical compound [Ti].CC(=O)CC(C)=O GYUPBLLGIHQRGT-UHFFFAOYSA-N 0.000 claims description 17
- 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
- 230000001476 alcoholic effect Effects 0.000 claims description 15
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 14
- 230000004044 response Effects 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 12
- 230000035484 reaction time Effects 0.000 claims description 3
- 238000006555 catalytic reaction Methods 0.000 abstract description 19
- 230000001699 photocatalysis Effects 0.000 abstract description 17
- 239000000463 material Substances 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 9
- 238000000034 method Methods 0.000 abstract description 9
- 239000012535 impurity Substances 0.000 abstract description 6
- RYSXWUYLAWPLES-MTOQALJVSA-N (Z)-4-hydroxypent-3-en-2-one titanium Chemical compound [Ti].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O RYSXWUYLAWPLES-MTOQALJVSA-N 0.000 abstract 1
- 238000010923 batch production Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 239000008204 material by function Substances 0.000 abstract 1
- 238000004659 sterilization and disinfection Methods 0.000 abstract 1
- 239000002351 wastewater Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 18
- 238000007146 photocatalysis Methods 0.000 description 15
- 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 12
- 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
- 238000001179 sorption measurement Methods 0.000 description 6
- 238000002798 spectrophotometry method Methods 0.000 description 6
- 238000003756 stirring 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
- 238000001816 cooling Methods 0.000 description 5
- 238000011156 evaluation Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 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
- 238000001354 calcination Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008859 change Effects 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
- 239000000314 lubricant Substances 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
- 238000011160 research Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000006467 substitution reaction Methods 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
-
- 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
-
- 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
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- 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
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- 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
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- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
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Abstract
The invention belongs to the technical field of functional materials, and relates to a preparation method of a nickel titanate/titanium dioxide composite nanomaterial. The method comprises the following steps: dissolving and uniformly mixing nickel acetylacetonate and titanium acetylacetonate in an alcohol solution, carrying out a cross-linking reaction at a certain temperature, and carrying out heat treatment in a muffle furnace to obtain the nickel titanate/titanium dioxide composite nanomaterial. The preparation method is simple and easy, and the nickel titanate/titanium dioxide composite nanomaterial has the advantages of high purity, low content of impurities, low preparation cost, excellent performances, and realization of industrial batch production. The nickel titanate/titanium dioxide composite nanomaterial prepared in the invention has high catalysis activity as a photocatalytic material, and has wide application prospects in the field of degradation of dye wastewater and indoor harmful gases and the field of photocatalytic disinfection.
Description
Technical field
The invention belongs to the preparing technical field of functional material, concretely relate to the preparation method of a kind of nickel titanate/titanium dioxide composite nano material.
Background technology
Nickel titanate (NiTiO3) belong to the trigonal system of ilmenite structure, for widely used inorganic functional material, in many industrial circles, there is application.Nickel titanate has high q-factor, low-k and good sound-optical and electrical-optical character, also has semiconduction and weak magnetic, is widely used as semiconductor rectifier, the catalyst of bicarbonate and surface coated dyeing intermixture.In addition, nickel titanate can also be used as high temperature under conditions of not having fluid lubricant and reduce friction and the covering material of loss.Additionally, nickel titanate is as the semi-conducting material of a kind of narrow band gap (2.18eV), there is good photoresponse in visible region, in terms of photocatalysis, have tempting application prospect.Titanium dioxide is stable chemical nature, active high, nontoxic, the cheap catalysis material of catalysis.But the energy gap of titanium dioxide (3.2 eV) is wider, and the utilization ratio for solar energy is relatively low.Utilizing two kinds of catalysis materials to be combined with each other, to be prepared as the method for composite be to improve a kind of effective way of conductor photocatalysis activity.Nickel titanate and titanium dioxide are combined with each other and prepare composite nano materials by the present invention.
Traditional prepares composite nano materials method, including solid sintering technology, coprecipitation, sol-gal process etc..These processes need complicated operation, and too high reaction temperature, long-time sintering process can make particle from caking, obtains the pattern that product is not fixed.Exploitation efficiently controls the pattern of nano material has important effect with structure to performances such as improving the optics of nano material, catalysis.
Summary of the invention
It is contemplated that provide a kind of preparation cost low in place of overcoming the deficiencies in the prior art, easily operated control, purpose product yield is high, homogeneity is good, and there is the preparation method of the nickel titanate/titanium dioxide composite nano material of higher catalytic activity, it is achieved that the technical process of composite nano materials powder body is produced in Low Temperature Solid-Phase calcining.By organizing contrast test, find that cross-linking reaction plays an important role in preparation technology more.Prepared nickel titanate/titanium dioxide composite nano material, has good photocatalysis performance, and under the process conditions of photocatalytic degradation of dye, within 60 minutes, degradation rate has reached more than 96%.Preparation method of the present invention can be applied equally to the chemosynthesis research of other functional material, and has broad application prospects.
For reaching above-mentioned purpose, the present invention is realized in.
A kind of preparation method of nickel titanate/titanium dioxide composite nano material, it is by nickel acetylacetonate and titanium acetylacetone, after dissolving mix homogeneously in alcoholic solution, carry out cross-linking reaction at a certain temperature, after the pyroreaction that continues, at a temperature of be down to room temperature, obtain purpose product.
As a kind of preferred version, the mol ratio of nickel acetylacetonate of the present invention and titanium acetylacetone is 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 more mixture in ethanol, ethylene glycol, isopropanol.
Further, cross-linking reaction temperature of the present invention is at 150～400 ° of C, and cross-linking reaction time is 2～8 h.
Further, pyroreaction temperature of the present invention is at 600～1000 ° of C, and the response time is 6～24 h.
Compared with prior art, the present invention has following features.
(1) present invention develops and prepares nickel titanate/titanium dioxide composite nano material new technology route, and product cut size is between 50～100nm.This technique preparation cost is low, easy to control, has higher production efficiency, it is possible to achieve industrial mass production.
(2) purpose product yield (99.0%～99.6%), product purity high (99.6%～99.8%) can meet the industrial application requirement to catalysis material product.
(3) purpose product nickel titanate/titanium dioxide composite nano material that prepared by the present invention is catalysis material, and within 60 minutes, degradation rate can reach (99.5%～97.0%), has higher catalysis activity.
Accompanying drawing explanation
The invention will be further described with detailed description of the invention below in conjunction with the accompanying drawings.Protection scope of the present invention is not only limited to the statement of following content.
Fig. 1 is the nickel titanate/titanium dioxide composite nano material SEM figure of the present invention.
Fig. 2 is the nickel titanate/titanium dioxide composite nano material SEM figure of the present invention.
Fig. 3 is the nickel titanate/titanium dioxide composite nano material SEM figure of the present invention.
Fig. 4 is the nickel titanate/titanium dioxide composite nano material X-ray diffractogram of the present invention.
Detailed description of the invention
The present invention designs a kind of chemical preparation process, prepares nickel titanate/titanium dioxide composite nano material by new chemistry route.Its photocatalysis property can be estimated by the typical methyl orange of photocatalytic degradation.
The present invention, with nickel acetylacetonate and titanium acetylacetone, is dissolved after mix homogeneously in alcoholic solution, is carried out cross-linking reaction at a certain temperature, after the pyroreaction that continues, at a temperature of be down to room temperature, obtain purpose product.
Preparation process of the present invention is.
(1) by nickel acetylacetonate and titanium acetylacetone, dissolving mix homogeneously in alcoholic solution, the mol ratio of nickel acetylacetonate and titanium acetylacetone is 1: 0.2～5；Nickel acetylacetonate molar concentration in alcoholic solution is 0.02～1.0 mol/L；Alcoholic solution is methanol, one or more mixture in ethanol, ethylene glycol, isopropanol.
(2) by the mixed solution that obtains at a certain temperature, carrying out cross-linking reaction, cross-linking reaction temperature is at 150～400 ° of C, and cross-linking reaction time is 2～8 h.
(3) cross-linking reaction terminates, then carries out high-temperature calcination, and pyroreaction temperature is at 600～1000 ° of C, and the response time is 6～24 h, at a temperature of be down to room temperature, obtain purpose product.
(4) nickel titanate/titanium dioxide composite nano material prepared by utilization is as photocatalyst (0.2g/L), the methyl orange solution of degraded 20mg/L.In photocatalysis experiment, light source used is 500W mercury lamp.Before irradiation, the methyl orange solution containing catalysis material stirs 30 minutes in the dark, carries out illumination after reaching adsorption equilibrium.By spectrophotometric determination methyl orange dye concentration change.
See shown in Fig. 1～3, for the nickel titanate/titanium dioxide composite nano material SEM figure of the present invention, it can be seen that product is the preferable nanoparticle of homogeneity.Fig. 4 is the nickel titanate/titanium dioxide composite nano material X-ray diffractogram of the present invention, and wherein # is the diffraction maximum of nickel titanate, and * is the diffraction maximum of titanium dioxide.
Embodiment 1.
The aqueous isopropanol that concentration is 0.2 mol/L nickel acetylacetonate is slowly dropped to concentration is 0.2
In the aqueous isopropanol of the titanium acetylacetone of mol/L, alcoholic solution dissolves mix homogeneously.The mixed solution obtained is carried out cross-linking reaction, and reaction temperature is 200
° C, the response time is 4 hours, and wherein the mol ratio of nickel acetylacetonate and titanium acetylacetone is 1: 2.After cross-linking reaction terminates, being connected in Muffle furnace and carry out pyroreaction, pyroreaction temperature is 600
° C, the response time is 24
h.After natural cooling, i.e. obtain purpose product.
Product cut size is between 50～70nm, and the yield of product is 99.6%.Product purity is 99.8%, impurity content: carbon is less than 0.2%.Nickel titanate/titanium dioxide composite nano material prepared by utilization is as photocatalyst (0.2g/L), the methyl orange solution of degraded 20mg/L.In photocatalysis experiment, light source used is 500W mercury lamp.Before irradiation, the methyl orange solution containing catalysis material stirs 30 minutes in the dark, carries out illumination after reaching adsorption equilibrium.By spectrophotometric determination methyl orange dye concentration, calculate degradation rate.In the test of photocatalysis evaluation catalysis activity, the degradation rate of 60 minutes is 99.5%.
Embodiment 2.
The methanol solution that concentration is 0.2 mol/L nickel acetylacetonate is slowly dropped to concentration is 0.2
The methanol solution of the titanium acetylacetone of mol/L, dissolves mix homogeneously in alcoholic solution.The mixed solution obtained is carried out cross-linking reaction, and reaction temperature is at 300 ° of C, and the response time is 8 hours, and wherein the mol ratio of nickel acetylacetonate and titanium acetylacetone is 1: 2.After cross-linking reaction terminates, being connected in Muffle furnace and carry out pyroreaction, pyroreaction temperature is 1000
° C, the response time is 6
h.After natural cooling, i.e. obtain purpose product.
Product cut size is between 60～80nm, and the yield of product is 99.2%.Product purity is not less than 99.7%, impurity content: carbon is less than 0.3%.Nickel titanate/titanium dioxide composite nano material prepared by utilization is as photocatalyst (0.2g/L), the methyl orange solution of degraded 20mg/L.In photocatalysis experiment, light source used is 500W mercury lamp.Before irradiation, the methyl orange solution containing catalysis material stirs 30 minutes in the dark, carries out illumination after reaching adsorption equilibrium.By spectrophotometric determination methyl orange dye concentration, calculate degradation rate.In the test of photocatalysis evaluation catalysis activity, the degradation rate of 60 minutes is 98.5%.
Embodiment 3.
The ethanol solution that concentration is 0.02 mol/L nickel acetylacetonate is slowly dropped to concentration is 0.02
The ethanol solution of the titanium acetylacetone of mol/L, dissolves mix homogeneously in alcoholic solution.The mixed solution obtained is carried out cross-linking reaction, and reaction temperature is 150
° C, the response time is 8 hours, and wherein the mol ratio of nickel acetylacetonate and titanium acetylacetone is 1: 2.After cross-linking reaction terminates, being connected in Muffle furnace and carry out pyroreaction, pyroreaction temperature is 1000
° C, the response time is 6
h.After natural cooling, i.e. obtain purpose product.
Product cut size is between 60～70nm, and the yield of product is 99.5%.Product purity is not less than 99.6%, impurity content: carbon is less than 0.4%.Nickel titanate/titanium dioxide composite nano material prepared by utilization is as photocatalyst (0.2g/L), the methyl orange solution of degraded 20mg/L.In photocatalysis experiment, light source used is 500W mercury lamp.Before irradiation, the methyl orange solution containing catalysis material stirs 30 minutes in the dark, carries out illumination after reaching adsorption equilibrium.By spectrophotometric determination methyl orange dye concentration, calculate degradation rate.In the test of photocatalysis evaluation catalysis activity, the degradation rate of 60 minutes is 97.8%.
Embodiment 4.
The aqueous isopropanol that concentration is 0.1 mol/L nickel acetylacetonate is slowly dropped to concentration is 0.1
The aqueous isopropanol of the titanium acetylacetone of mol/L, dissolves mix homogeneously in alcoholic solution.The mixed solution obtained is carried out cross-linking reaction, and reaction temperature is at 400 ° of C, and the response time is 4 hours, and wherein the mol ratio of nickel acetylacetonate and titanium acetylacetone is 1: 2.After cross-linking reaction terminates, being connected in Muffle furnace and carry out pyroreaction, pyroreaction temperature is 800
° C, the response time is 10
h.After natural cooling, i.e. obtain purpose product.
Product cut size is between 80～100nm, and the yield of product is 99.5%.Product purity is not less than 99.7%, impurity content: carbon is less than 0.3%.Nickel titanate/titanium dioxide composite nano material prepared by utilization is as photocatalyst (0.2g/L), the methyl orange solution of degraded 20mg/L.In photocatalysis experiment, light source used is 500W mercury lamp.Before irradiation, the methyl orange solution containing catalysis material stirs 30 minutes in the dark, carries out illumination after reaching adsorption equilibrium.By spectrophotometric determination methyl orange dye concentration, calculate degradation rate.In the test of photocatalysis evaluation catalysis activity, the degradation rate of 60 minutes is 99.4%.
Embodiment 5.
The ethylene glycol solution that concentration is 0.02 mol/L nickel acetylacetonate is slowly dropped to concentration is 0.02
In the ethylene glycol solution of the titanium acetylacetone of mol/L, alcoholic solution dissolves mix homogeneously.The mixed solution obtained is carried out cross-linking reaction, and reaction temperature is 300
° C, the response time is 8 hours, and wherein the mol ratio of nickel acetylacetonate and titanium acetylacetone is 1: 2.After cross-linking reaction terminates, being connected in Muffle furnace and carry out pyroreaction, pyroreaction temperature is 1000
° C, the response time is 12
h.After natural cooling, i.e. obtain purpose product.
Product cut size is between 60～100nm, and the yield of product is 99.5%.Product purity is not less than 99.6%, impurity content: carbon is less than 0.4%.Nickel titanate/titanium dioxide composite nano material prepared by utilization is as photocatalyst (0.2g/L), the methyl orange solution of degraded 20mg/L.In photocatalysis experiment, light source used is 500W mercury lamp.Before irradiation, the methyl orange solution containing catalysis material stirs 30 minutes in the dark, carries out illumination after reaching adsorption equilibrium.By spectrophotometric determination methyl orange dye concentration, calculate degradation rate.In the test of photocatalysis evaluation catalysis activity, the degradation rate of 60 minutes is 97.0%.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.All within the spirit and principles in the present invention, any modification, equivalent substitution and improvement etc. made, should be included within the scope of the present invention.
Claims (6)
1. the preparation method of nickel titanate/titanium dioxide composite nano material, it is characterised in that by nickel acetylacetonate and titanium acetylacetone, after dissolving mix homogeneously in alcoholic solution, carry out cross-linking reaction at a certain temperature, after the pyroreaction that continues, at a temperature of be down to room temperature, obtain purpose product.
The preparation method of nickel titanate/titanium dioxide composite nano material the most according to claim 1, it is characterised in that: described nickel acetylacetonate and the mol ratio of titanium acetylacetone are 1: 0.2～5.
The preparation method of nickel titanate/titanium dioxide composite nano material the most according to claim 2, it is characterised in that: described nickel acetylacetonate molar concentration in alcoholic solution is 0.02～1.0 mol/L.
The preparation method of nickel titanate/titanium dioxide composite nano material the most according to claim 3, it is characterised in that: described alcoholic solution is methanol, one or more mixture in ethanol, ethylene glycol, isopropanol.
The preparation method of nickel titanate/titanium dioxide composite nano material the most according to claim 4, it is characterised in that: described cross-linking reaction temperature is at 150～400 ° of C, and cross-linking reaction time is 2～8 h.
The preparation method of nickel titanate/titanium dioxide composite nano material the most according to claim 5, it is characterised in that: described pyroreaction temperature is at 600～1000 ° of C, and the response time is 6～24 h.
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Cited By (6)
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| CN106241853A (en) * | 2016-09-12 | 2016-12-21 | 渤海大学 | A kind of preparation method of yittrium oxide nano material |
| CN106348344A (en) * | 2016-09-12 | 2017-01-25 | 渤海大学 | Preparation method of lanthanum chromite nano material |
| CN106348342A (en) * | 2016-09-12 | 2017-01-25 | 渤海大学 | Spherical lanthanum zirconate nano material preparation method |
| CN107029731A (en) * | 2017-04-27 | 2017-08-11 | 华南理工大学 | A kind of La doped NiTi compound oxide photocatalyst and its application in photochemical catalytic oxidation desulfurization |
| CN108452805A (en) * | 2017-02-17 | 2018-08-28 | 中国科学院福建物质结构研究所 | A kind of NiTiO for photodissociation aquatic products hydrogen3/TiO2Catalyst and its preparation method and application |
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| CN106348344B (en) * | 2016-09-12 | 2018-03-20 | 渤海大学 | A kind of preparation method of Lanthanum Chromite 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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| CN107029731A (en) * | 2017-04-27 | 2017-08-11 | 华南理工大学 | A kind of La doped NiTi compound oxide photocatalyst and its application in photochemical catalytic oxidation desulfurization |
| CN107029731B (en) * | 2017-04-27 | 2019-10-18 | 华南理工大学 | A kind of La doped NiTi compound oxide photocatalyst and its application in photochemical catalytic oxidation desulfurization |
| CN110407260A (en) * | 2019-08-29 | 2019-11-05 | 江苏师范大学 | A kind of rodlike NiTiO of Porous hollow3/A-TiO2/R-TiO2Compound and its synthetic method |
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