CN108906020A - A kind of preparation method of titanium dioxide-zinc oxide composite catalyzing material - Google Patents

A kind of preparation method of titanium dioxide-zinc oxide composite catalyzing material Download PDF

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Publication number
CN108906020A
CN108906020A CN201810811403.2A CN201810811403A CN108906020A CN 108906020 A CN108906020 A CN 108906020A CN 201810811403 A CN201810811403 A CN 201810811403A CN 108906020 A CN108906020 A CN 108906020A
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titanium dioxide
zinc oxide
catalyzing material
composite catalyzing
oxide composite
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陆伟
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Zhangjiagang City Department Of Dingxin Mstar Technology Ltd
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Zhangjiagang City Department Of Dingxin Mstar Technology Ltd
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    • 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
    • B01J23/06Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of zinc, cadmium or mercury
    • 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
    • B01J23/002Mixed oxides other than spinels, e.g. perovskite
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/30Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39Photocatalytic properties
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08Heat treatment
    • B01J37/10Heat treatment in the presence of water, e.g. steam

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
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Abstract

The invention discloses a kind of preparation methods of titanium dioxide-zinc oxide composite catalyzing material, including:(1) by nano titanium dioxide powder be added volume be 1:In 2 dehydrated alcohol and the mixed solution of deionized water, 1~2h of ultrasonic reaction makes it be uniformly dispersed, and obtains the titanium dioxide suspension that concentration is 0.1~0.5g/L;(2) under stirring conditions, the ethanol solution of soluble zinc salt is added into above-mentioned titanium dioxide suspension, stirs 20~30min, adding ammonium hydroxide liquid and adjusting pH value is 8~9, continues to be stirred to react 30~40min under 60~80 DEG C of water bath conditions;(3) product obtained in step (2) is filtered, after gained Washing of Filter Cake to neutrality, in 80~120 DEG C of dry 1~2h, 3~5h is roasted at 300~500 DEG C, obtains titanium dioxide-zinc oxide composite catalyzing material.In the present invention, by titanium dioxide doping zinc-oxide help to improve the light degradation activity of composite catalyzing material, to increase to the absorptivity of ultraviolet light.

Description

A kind of preparation method of titanium dioxide-zinc oxide composite catalyzing material
Technical field
The present invention relates to field of material technology, more particularly to a kind of system of titanium dioxide-zinc oxide composite catalyzing material Preparation Method.
Background technique
Environmental pollution and energy resources anxiety are the serious problems that future social development has to face.Hydrogen is a kind of It cleans, is efficient, reproducible energy carrier, being widely used in national economy and social life.Due to solar energy Development and utilization with enriching for water resource, solar energy photocatalytic hydrogen manufacturing have very big development potentiality.In recent years, nanometer titanium dioxide Titanium (TiO2) due to the advantage of its excellent photocatalysis performance, chemical stability height, anti-light corrosion are nontoxic, low in cost etc. excellent Point, it is considered to be most promising catalysis material causes the extensive concern of people.Especially with one-dimensional nano structure Nano-TiO2Material, large specific surface area, length-width ratio are big, and surface-active site is more, and the fast feature of electron transfer rate makes it Possess higher photocatalytic activity.However, due to TiO2Band gap it is relatively wide (3.2eV) so that it is only in response to ultraviolet waves Long light irradiation.In addition, photo-generate electron-hole is in the transition process from inside to surface during Photocatalyzed Hydrogen Production In be easy catalytic inner recombinate, cause solar energy to be converted into the poor efficiency of Hydrogen Energy.In the past few decades, researcher Various methods have been researched and developed to improve TiO2Photocatalysis efficiency, including noble metal loading, metal and nonmetalloid are mixed It miscellaneous (such as N and S element), dye sensitization and is coupled etc. with other semiconductors.In recent years, metal oxide (such as CuO, ZnO, NiO), due to the greater activity showed in terms of photochemical catalyzing, cause the concern of researchers.
Zinc oxide (ZnO) possesses biggish sharp since it is the direct band-gap semicondictor of greater band gap (3.37eV) Sub- binding energy (60meV), it is considered to be up-and-coming photoelectric material is frequently used to do photoelectric, while also applying The electrode material of material, solar battery and Li-Ion rechargeable battery in terms of laser diode.ZnO has and TiO2It is similar Band structure and physical property, but simultaneously also have the unexistent characteristic of some titanium dioxide, such as higher quantum yield and Higher electron mobility, this is advantageous to improve its photocatalytic activity.In addition, nano-ZnO have easily crystallization and it is each to different Property growth performance, this allows nano-ZnO to be easy to be synthesized the nanostructures of different morphologies.Importantly, the valence band location of ZnO and Stronger electronics rate travel is conducive to water decomposition hydrogen.Meanwhile ZnO and TiO2Band structure can be good at matching. Therefore, nano zine oxide is coupled on one-dimensional nanometer titanic oxide material, is expected to improve its photocatalytic activity and produces hydrogen Energy.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of titanium dioxide-zinc oxide composite catalyzing material, to overcome Deficiency in the prior art.
To achieve the above object, the present invention provides the following technical solutions:
A kind of preparation method of titanium dioxide-zinc oxide composite catalyzing material, including:
(1) by nano titanium dioxide powder be added volume be 1:In 2 dehydrated alcohol and the mixed solution of deionized water, 1~2h of ultrasonic reaction, makes it be uniformly dispersed, and obtains the titanium dioxide suspension that concentration is 0.1~0.5g/L;
(2) under stirring conditions, the ethanol solution of soluble zinc salt, stirring are added into above-mentioned titanium dioxide suspension 20~30min, adding ammonium hydroxide liquid and adjusting pH value is 8~9, continue to be stirred to react 30 under 60~80 DEG C of water bath conditions~ 40min;
(3) product obtained in step (2) is filtered, after gained Washing of Filter Cake to neutrality, in 80~120 DEG C of dryings 1~2h roasts 3~5h at 300~500 DEG C, obtains titanium dioxide-zinc oxide composite catalyzing material.
Preferably, in step (1), the concentration of the titanium dioxide suspension is 0.3g/L.
Preferably, in step (2), the concentration of the soluble zinc salt is 0.1~1.0mol/L.
Preferably, the soluble zinc salt is zinc acetate or zinc nitrate.
Preferably, in step (2), the concentration of the ammonium hydroxide is 0.5~2.0mol/L.
Preferably, in step (3), the heating rate of the roasting is 5~10 DEG C/min.
Preferably, in the titanium dioxide-zinc oxide composite catalyzing material, the mass fraction of the titanium dioxide is 78~ 85%, the mass fraction of the zinc oxide is 15~22%.
Compared with the prior art, the advantages of the present invention are as follows:In the present invention, by titanium dioxide doping zinc-oxide have The light degradation activity for helping improve composite catalyzing material, to increase the absorptivity to ultraviolet light.
Specific embodiment
The present invention is described further by the following example:According to following embodiments, the present invention may be better understood. However, as it will be easily appreciated by one skilled in the art that specific material ratio, process conditions and its result described in embodiment are only used In illustrating the present invention, without the present invention described in detail in claims should will not be limited.
The present invention discloses a kind of preparation method of titanium dioxide-zinc oxide composite catalyzing material, including:
(1) by nano titanium dioxide powder be added volume be 1:In 2 dehydrated alcohol and the mixed solution of deionized water, 1~2h of ultrasonic reaction, makes it be uniformly dispersed, and obtains the titanium dioxide suspension that concentration is 0.1~0.5g/L;
(2) under stirring conditions, the ethanol solution of soluble zinc salt, stirring are added into above-mentioned titanium dioxide suspension 20~30min, adding ammonium hydroxide liquid and adjusting pH value is 8~9, continue to be stirred to react 30 under 60~80 DEG C of water bath conditions~ 40min;
(3) product obtained in step (2) is filtered, after gained Washing of Filter Cake to neutrality, in 80~120 DEG C of dryings 1~2h roasts 3~5h at 300~500 DEG C, obtains titanium dioxide-zinc oxide composite catalyzing material.
Wherein, the concentration of the titanium dioxide suspension is 0.3g/L.
Wherein, the soluble zinc salt is zinc acetate or zinc nitrate, the concentration of the soluble zinc salt is 0.1~ 1.0mol/L, it is preferred that the concentration of the soluble zinc salt is 0.5mol/L.
Wherein, the concentration of the ammonium hydroxide is 0.5~2.0mol/L, it is preferred that the concentration of the ammonium hydroxide is 1.5mol/L.
Wherein, the heating rate of the roasting be 5~10 DEG C/min, it is preferred that the heating rate of the roasting be 8 DEG C/ min。
In the titanium dioxide-zinc oxide composite catalyzing material according to made from the above method, the quality point of the titanium dioxide Number is 78~85%, and the mass fraction of the zinc oxide is 15~22%.
Following preparation sides that titanium dioxide-zinc oxide composite catalyzing material in the present invention is illustrated with specifically embodiment Method.
Embodiment 1
(1) by nano titanium dioxide powder be added volume be 1:In 2 dehydrated alcohol and the mixed solution of deionized water, Ultrasonic reaction 1h, makes it be uniformly dispersed, and obtains the titanium dioxide suspension that concentration is 0.1g/L;
(2) under stirring conditions, it is 0.1mol/L acetic acid zinc salt that concentration is added into above-mentioned titanium dioxide suspension Ethanol solution, stir 20min, add concentration be 0.5mol/L ammonium hydroxide liquid adjust pH value be 8, continue under 60 DEG C of water bath conditions It is stirred to react 30min;
(3) product obtained in step (2) is filtered, after gained Washing of Filter Cake to neutrality, in 80 DEG C of dry 1h, then 3h is roasted at 300 DEG C, wherein the heating rate of roasting is 5 DEG C/min, obtains titanium dioxide-zinc oxide composite catalyzing material.
In the titanium dioxide-zinc oxide composite catalyzing material according to made from the above method, the quality point of the titanium dioxide Number is 78%, and the mass fraction of the zinc oxide is 22%.
Embodiment 2
(1) by nano titanium dioxide powder be added volume be 1:In 2 dehydrated alcohol and the mixed solution of deionized water, Ultrasonic reaction 1.5h, makes it be uniformly dispersed, and obtains the titanium dioxide suspension that concentration is 0.3g/L;
(2) under stirring conditions, it is 0.5mol/L acetic acid zinc salt that concentration is added into above-mentioned titanium dioxide suspension Ethanol solution, stir 25min, add concentration be 1.5mol/L ammonium hydroxide liquid adjust pH value be 8.5, under 70 DEG C of water bath conditions after It is continuous to be stirred to react 35min;
(3) product obtained in step (2) is filtered, after gained Washing of Filter Cake to neutrality, in 100 DEG C of dryings 1.5h roasts 4h at 400 DEG C, wherein the heating rate of roasting is 8 DEG C/min, obtains that titanium dioxide-zinc oxide is compound to urge Change material.
In the titanium dioxide-zinc oxide composite catalyzing material according to made from the above method, the quality point of the titanium dioxide Number is 80%, and the mass fraction of the zinc oxide is 20%.
Embodiment 3
(1) by nano titanium dioxide powder be added volume be 1:In 2 dehydrated alcohol and the mixed solution of deionized water, Ultrasonic reaction 2h, makes it be uniformly dispersed, and obtains the titanium dioxide suspension that concentration is 0.5g/L;
(2) under stirring conditions, it is 1.0mol/L acetic acid zinc salt that concentration is added into above-mentioned titanium dioxide suspension Ethanol solution, stir 30min, add concentration be 2.0mol/L ammonium hydroxide liquid adjust pH value be 9, continue under 80 DEG C of water bath conditions It is stirred to react 40min;
(3) product obtained in step (2) is filtered, after gained Washing of Filter Cake to neutrality, in 120 DEG C of dry 2h, 5h is roasted at 500 DEG C, wherein the heating rate of roasting is 10 DEG C/min, obtains titanium dioxide-zinc oxide composite catalyzing material Material.
In the titanium dioxide-zinc oxide composite catalyzing material according to made from the above method, the quality point of the titanium dioxide Number is 85%, and the mass fraction of the zinc oxide is 15%.
In the present invention, lived by the light degradation that doping zinc-oxide helps to improve composite catalyzing material in titanium dioxide Property, to increase the absorptivity to ultraviolet light;After ultraviolet light waste water 60min, the degradation rate of organic matter is up to 98.6%.Therefore, the composite catalyzing material in the present invention has broad application prospects in terms of photocatalysis.
Finally, it is to be noted that, the terms "include", "comprise" or its any other variant be intended to it is non-exclusive Property include so that include a series of elements process, method, article or equipment not only include those elements, but also Further include other elements that are not explicitly listed, or further include for this process, method, article or equipment it is intrinsic Element.

Claims (7)

1. a kind of preparation method of titanium dioxide-zinc oxide composite catalyzing material, which is characterized in that including:
(1) by nano titanium dioxide powder be added volume be 1:In 2 dehydrated alcohol and the mixed solution of deionized water, ultrasound 1~2h is reacted, it is made to be uniformly dispersed, obtains the titanium dioxide suspension that concentration is 0.1~0.5g/L;
(2) under stirring conditions, into above-mentioned titanium dioxide suspension be added soluble zinc salt ethanol solution, stirring 20~ 30min, adding ammonium hydroxide liquid and adjusting pH value is 8~9, continues to be stirred to react 30~40min under 60~80 DEG C of water bath conditions;
(3) product obtained in step (2) is filtered, after gained Washing of Filter Cake to neutrality, 80~120 DEG C dry 1~ 2h roasts 3~5h at 300~500 DEG C, obtains titanium dioxide-zinc oxide composite catalyzing material.
2. the preparation method of titanium dioxide-zinc oxide composite catalyzing material according to claim 1, which is characterized in that step Suddenly in (1), the concentration of the titanium dioxide suspension is 0.3g/L.
3. the preparation method of titanium dioxide-zinc oxide composite catalyzing material according to claim 1, which is characterized in that step Suddenly in (2), the concentration of the soluble zinc salt is 0.1~1.0mol/L.
4. the preparation method of titanium dioxide-zinc oxide composite catalyzing material according to claim 3, which is characterized in that institute Stating soluble zinc salt is zinc acetate or zinc nitrate.
5. the preparation method of titanium dioxide-zinc oxide composite catalyzing material according to claim 1, which is characterized in that step Suddenly in (2), the concentration of the ammonium hydroxide is 0.5~2.0mol/L.
6. the preparation method of titanium dioxide-zinc oxide composite catalyzing material according to claim 1, which is characterized in that step Suddenly in (3), the heating rate of the roasting is 5~10 DEG C/min.
7. the preparation method of titanium dioxide-zinc oxide composite catalyzing material according to claim 1, which is characterized in that institute It states in titanium dioxide-zinc oxide composite catalyzing material, the mass fraction of the titanium dioxide is 78~85%, the zinc oxide Mass fraction is 15~22%.
CN201810811403.2A 2018-07-23 2018-07-23 A kind of preparation method of titanium dioxide-zinc oxide composite catalyzing material Withdrawn CN108906020A (en)

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CN110142050A (en) * 2019-05-27 2019-08-20 吕梁学院 The preparation method of zinc sulphide doped titanium dioxide photocatalyst
CN110947383A (en) * 2019-11-12 2020-04-03 芜湖职业技术学院 Polyester fiber photodegradation catalyst and preparation method thereof
CN111974375A (en) * 2020-08-28 2020-11-24 嘉兴学院 Composite photocatalyst film and preparation method and application thereof
CN114590834A (en) * 2022-03-30 2022-06-07 广州天赐高新材料股份有限公司 Nano titanium dioxide-zinc oxide hybrid material and synthetic method thereof

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109731617A (en) * 2018-12-13 2019-05-10 东莞理工学院 A kind of Fe3O4/ polypyrrole/polyaniline/TiO2The preparation method of/ZnO composite material
CN110142050A (en) * 2019-05-27 2019-08-20 吕梁学院 The preparation method of zinc sulphide doped titanium dioxide photocatalyst
CN110947383A (en) * 2019-11-12 2020-04-03 芜湖职业技术学院 Polyester fiber photodegradation catalyst and preparation method thereof
CN111974375A (en) * 2020-08-28 2020-11-24 嘉兴学院 Composite photocatalyst film and preparation method and application thereof
CN114590834A (en) * 2022-03-30 2022-06-07 广州天赐高新材料股份有限公司 Nano titanium dioxide-zinc oxide hybrid material and synthetic method thereof

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Application publication date: 20181130