CN105905940A - Preparation method of nickel titanate/titanium dioxide composite nanomaterial - Google Patents

Preparation method of nickel titanate/titanium dioxide composite nanomaterial Download PDF

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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
nickel
preparation
nickel titanate
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CN105905940B (en
Inventor
许家胜
艾慧婷
张�杰
张霞
王莉丽
王琳
孙誉东
李阁
唐爽
丁亮
车昕彤
刘娇
邢锦娟
张艳萍
刘琳
钱建华
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Bohai University
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00Compounds of titanium
    • C01G23/04Oxides; Hydroxides
    • C01G23/047Titanium dioxide
    • C01G23/053Producing by wet processes, e.g. hydrolysing titanium salts
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/74Iron group metals
    • B01J23/755Nickel
    • B01J35/39
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-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
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/64Nanometer sized, i.e. from 1-100 nanometer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

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

A kind of preparation method of nickel titanate/titanium dioxide composite nano material
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)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106241853A (en) * 2016-09-12 2016-12-21 渤海大学 A kind of preparation method of yittrium oxide nano material
CN106348342A (en) * 2016-09-12 2017-01-25 渤海大学 Spherical lanthanum zirconate nano material preparation method
CN106348344A (en) * 2016-09-12 2017-01-25 渤海大学 Preparation method of lanthanum chromite nano material
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
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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CN103531756A (en) * 2013-11-01 2014-01-22 北京化工大学 Carbon nanofiber loaded lithium titanate thin film materials and manufacturing method thereof
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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
CN106348342A (en) * 2016-09-12 2017-01-25 渤海大学 Spherical lanthanum zirconate nano material preparation method
CN106348344A (en) * 2016-09-12 2017-01-25 渤海大学 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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