CN102240540B - Flaky gallium-containing nano photocatalyst and use thereof in light degradation of organic pollutants - Google Patents

Flaky gallium-containing nano photocatalyst and use thereof in light degradation of organic pollutants Download PDF

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CN102240540B
CN102240540B CN201110120513A CN201110120513A CN102240540B CN 102240540 B CN102240540 B CN 102240540B CN 201110120513 A CN201110120513 A CN 201110120513A CN 201110120513 A CN201110120513 A CN 201110120513A CN 102240540 B CN102240540 B CN 102240540B
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gallium
photocatalyst
sheet
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nano
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CN102240540A (en
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张法智
王雷
赵晓非
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Beijing University of Chemical Technology
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Beijing University of Chemical Technology
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    • Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy

Abstract

The invention discloses a flaky gallium-containing nano photocatalyst and use thereof in the light degradation of organic pollutants, which belong to the technical field of preparation of solid photocatalysts. In the invention, the flaky ZnO and ZnGa2O4 composite nano photocatalyst is prepared by high-temperature roasting of layered bishydroxy composite metal hydroxide precursor, namely a zinc/gallium hydrotalcite precursor. When the method provided by the invention is used to prepare a photocatalyst material, the preparation method is simple and convenient, a basic flaky structure is still kept after high-temperature roasting, the nano scale is large (the diameter is about 200 to 400 nanometers), and photocatalytic reaction is promoted.

Description

A kind of sheet contains the application of gallium nano-photocatalyst and light degradation organic pollution thereof
Technical field
The invention belongs to the solid photocatalysis field, be specifically related to contain gallium nano-photocatalyst and the application on the light degradation organic pollution thereof by a kind of sheet of hydrotalcite precursor roasting preparation.
Background technology
Find TiO from Japanese Fujishima in 1972 and Honda 2Since the monocrystalline photocatalysis brine electrolysis, the research of Nano semiconductor multiphase photocatalysis reaction aspect has obtained deeply carrying out widely.Through 30 years of researches, photocatalysis has all obtained bigger progress in following 4 fields: (1) surround lighting catalysis (comprise and dispose of sewage and purify air etc.); (2) conversion of solar energy photocatalysis (mainly being photocatalytic hydrogen production by water decomposition); (3) deodorization and sterilization; (4) dye sensitized nano crystal salar battery.
Houghite is claimed laminated dihydroxy composite metal hydroxide (Layered Double Hydroxide again; Be abbreviated as LDHs); Be an anionoid type layer structure functional material, its laminate is by positively charged cation composition, and interlayer is made up of the anion and the hydrone of balancing charge.The LDHs chemical composition has following general formula: [M II 1-xM III x(OH) 2] X+(A N-) X/nYH 2O, wherein M IICan be " Mg 2+, Zn 2+, Ni 2+" wait divalent metal, M IIICan be " Al 3+, Cr 3+, Fe 3+" wait trivalent metal cation, be positioned on the main body laminate; A N-Be interlayer anion; X is M III/ (M II+ M III) molar ratio; Y is the number of intermediary water molecule.Be positioned at the divalent metal M on the laminate 2+Can be by the close trivalent metal cation M of ionic radius in certain proportion 3+The isomorphous replaces, thereby makes body layer strip positive charge partly; The object A that interlayer can exchange N-Anion and laminate positive charge balance each other, and therefore make this Subjective and Objective structure of LDHs present electroneutral.LDHs has body layer sheetmetal ion and forms design features such as the adjustable sex change in space in adjustable sex change, main body laminate charge density and the adjustable sex change that distributes, intercalant anion object kind and adjustable number sex change, the layer, the adjustable sex change of host-guest interaction.This special nature that on chemistry and structure, shows not only makes it have ion-exchange performance, all has in many fields such as catalysis, absorption, ion-exchange, electricity material, optical material, biosensor techniques very widely and uses.
Hydrotalcite-based compound is because of having extremely people's attention of special layer structure and character, and is widely used in catalytic field.In recent years, many scholar's research find that spinel oxide also can be used as catalysis material.The spinel-type compound is because its energy gap is little, and good stability is one type of photochemical catalyst with potential using value.Preparation method about spinelle is a lot, wherein is precursor calcining preparation spinelle with the hydrotalcite, and method is simple, easy operating, and stable performance is widely used.
People such as Anna Mclaren find that the zinc oxide of laminated structure helps generating the OH free radical on its surface, thereby help the photocatalytic degradation methylene blue when the shape and size effect of research single-crystal zinc-oxide.And people such as Nikolai Kislov have also obtained similar conclusion when research zinc oxide light degradation methyl orange.
Summary of the invention
The purpose of this invention is to provide a kind of sheet contains the gallium nano-photocatalyst and is applied to the light degradation organic pollution.The present invention uses single catalyst precarsor (ZnGa-LDHs) to make final catalyst through roasting: ZnO and ZnGa 2O 4Compound, this catalyst can the photocatalytic degradation methylene blues, kept the basic laminated structure of precursor, and (diameter is about 200～400nm), helps light-catalyzed reaction to have bigger nano-scale.
Concrete preparation process of the present invention is following:
A, preparation zinc gallium hydrotalcite precursor: take by weighing ZnCl 2And GaCl 3Be dissolved in and be made into mixing salt solution, wherein Zn in the deionized water 2+Concentration is 0.12～6mol/L, Zn 2+With Ga 3+Mol ratio is 2～4; And then take by weighing NaOH and Na 2CO 3Be dissolved in and be made into mixed ammonium/alkali solutions in the deionized water, wherein n (Na 2CO 3)/[n (Ga 3+)]=2.0～2.5, n (NaOH)/[n (Zn 2+)+n (Ga 3+)]=1.8～2.5, NaOH concentration is 1.0～6.0mol/L, n (NaOH), n (Zn 2+), n (Ga 3+), n (Na 2CO 3) be respectively NaOH, Zn 2+, Ga 3+, Na 2CO 3Molal quantity; Above-mentioned two kinds of mixed solutions are added drop-wise in the four-hole boiling flask simultaneously, and in the dropping process, keeping the pH value of reaction solution in the flask is 9～11, and after dropwising, keeping reaction temperature is 80～100 ℃, and backflow crystallization 12～36h obtains zinc gallium hydrotalcite precursor slurry; Zinc gallium hydrotalcite precursor slurry behind ℃ drying 24～48h of centrifuge washing to pH=7～8,60～80, promptly gets zinc gallium hydrotalcite;
B, the zinc gallium hydrotalcite that steps A is obtained are put into crucible; 600～900 ℃ of roasting 3～5h in Muffle furnace; Concrete scheme is: the Muffle furnace initial temperature is 15～30 ℃; Then with heating rate temperature programming to 700～900 of 5～10 ℃/min ℃, and then keep 3～5h, naturally cool to room temperature afterwards; After roasting finishes, the sheet that makes is contained the gallium nano-photocatalyst take out, put into drier and preserve.
The chemical general formula of the described zinc gallium of steps A hydrotalcite precursor is:
[Zn 1-xGa x(OH) 2] X+(CO 3) 2- X/2NH 2O, wherein, 0.2＜x＜0.33; N is the quantity of the crystallization water, 0.1＜n＜10.
It is ZnO and ZnGa that the described sheet of step B contains the gallium nano-photocatalyst 2O 4Compound, with still keeping laminated structure after its high-temperature roasting, the diameter of sheet is 200～400nm.
The sheet of step B preparation is contained the gallium nano-photocatalyst be applied to the photocatalytic degradation methylene blue.
The reaction condition of described photocatalytic degradation methylene blue is following: reaction pressure is a normal pressure, and reaction temperature is a room temperature, and the concentration of methylene blue in the aqueous solution is 1 * 10 -5～2 * 10 -5Mol/L; The quality that the sheet of adding step B preparation contains the gallium nano-photocatalyst is equivalent to 0.01～0.03% of system quality; Containing catalyst solution keeps 30～60min up to reaching the adsorption-desorption balance in advance under dark condition; Open light source, adopt magnetic stirring apparatus to stir reaction time 15～30min in the course of reaction.
Said light source is a CEL-LAM500 ultraviolet light long arc mercury lamp, and the mercury lamp input power is 500W, and total length is 200mm; Power supply is input as 220V 50Hz and exchanges; Other is furnished with photochemical reactor and cold-trap, and wherein the photochemical reactor model is CEPR250, and the cold-trap model is CEQW60.
The zinc gallium hydrotalcite precursor that the present invention uses has good crystal formation; The sheet that its roasting is obtained contains the gallium nano-photocatalyst and has good heat endurance; Still keep basic laminated structure after the high-temperature roasting; And (diameter is about 200～400nm), helps light-catalyzed reaction to have bigger nano-scale.
Description of drawings
Fig. 1 is the XRD spectra that embodiment 2 prepared sheets contain the gallium nano-photocatalyst;
Fig. 2 is the SEM image that embodiment 2 prepared sheets contain the gallium nano-photocatalyst;
Fig. 3 is a CEL-LAM500 mercury lamp lamp source installation drawing;
Fig. 4 is photocatalytic degradation methylene blue solution concentration and the light application time curve that embodiment 2 prepared sheets contain the gallium nano-photocatalyst.
The specific embodiment
Below in conjunction with embodiment the present invention is done further description:
Embodiment 1
A: take by weighing 10.90g ZnCl 2With 7.04g GaCl 3Be dissolved in and be made into the 100ml mixing salt solution in the deionized water; And then take by weighing 7.68g NaOH and 8.48g Na 2CO 3Be dissolved in and be made into the 100ml mixed ammonium/alkali solutions in the deionized water; Above-mentioned two kinds of mixed solutions are added drop-wise in the four-hole boiling flask of 500ml simultaneously, and in the dropping process, keeping the pH value of reaction solution in the flask is 10, and after dropwising, keeping reaction temperature is 80 ℃, and backflow crystallization 24h obtains zinc gallium hydrotalcite precursor slurry; Zinc gallium hydrotalcite precursor slurry to pH=8, behind the dry 24h, promptly gets zinc gallium hydrotalcite through centrifuge washing in 60 ℃ of electric heating constant temperature air dry ovens; B: the zinc gallium hydrotalcite of above-mentioned gained is put into crucible; 800 ℃ of roasting 4h in Muffle furnace, concrete scheme is: the Muffle furnace initial temperature is 25 ℃, then with the heating rate temperature programming to 800 of 10 ℃/min ℃; And then 800 ℃ of maintenance 4h, naturally cool to room temperature afterwards; After roasting finishes, the sheet that makes is contained the gallium nano-photocatalyst take out, put into drier and preserve.
The chemical general formula of the described zinc gallium of steps A hydrotalcite precursor is:
[Zn 1-xGa x(OH) 2] X+(CO 3) 2- X/2NH 2O, wherein, x=0.33; N is the quantity of the crystallization water, n=1.2.
It is ZnO and ZnGa that the sheet that step B makes contains the gallium nano-photocatalyst 2O 4Compound, with still keeping laminated structure after its high-temperature roasting, the diameter of sheet is 200～400nm.
Sheet with making contains gallium nano-photocatalyst photocatalytic degradation methylene blue: in photocatalytic reaction device, add 300ml 1 * 10 -5The mol/L methylene blue solution adds the catalyst that 0.03g step B makes, and keeps 30min under the half-light condition; After the adsorption equilibrium, open light source, magnetic agitation; A detection is got in segmentation, and whole process reaction pressure is normal pressure, and reaction temperature is a room temperature; Behind the reaction 15min, recording the methylene blue degradation rate is 98%.
Light source is a CEL-LAM500 ultraviolet light long arc mercury lamp, and the mercury lamp input power is 500W, and total length is 200mm, and power supply is input as 220V 50Hz and exchanges, and other is furnished with photochemical reactor and cold-trap, and wherein the photochemical reactor model is CEPR250, and the cold-trap model is CEQW60.
Embodiment 2
A: take by weighing 12.27g ZnCl 2With 5.28g GaCl 3Be dissolved in and be made into the 100ml mixing salt solution in the deionized water; And then take by weighing 7.68g NaOH and 6.36g Na 2CO 3Be dissolved in and be made into the 100ml mixed ammonium/alkali solutions in the deionized water; Above-mentioned two kinds of mixed solutions are added drop-wise in the four-hole boiling flask of 500ml simultaneously, and in the dropping process, keeping the pH value of reaction solution in the flask is 10, and after dropwising, keeping reaction temperature is 80 ℃, and backflow crystallization 24h obtains zinc gallium hydrotalcite precursor slurry; Zinc gallium hydrotalcite precursor slurry to pH=8, behind the dry 24h, promptly gets zinc gallium hydrotalcite through centrifuge washing in 60 ℃ of electric heating constant temperature air dry ovens;
B: with embodiment 1.
The chemical general formula of the described zinc gallium of steps A hydrotalcite precursor is:
[Zn 1-xGa x(OH) 2] X+(CO 3) 2- X/2NH 2O, wherein, x=0.25; N is the quantity of the crystallization water, n=1.4.
It is ZnO and ZnGa that the sheet that step B makes contains the gallium nano-photocatalyst 2O 4Compound, with still keeping laminated structure after its high-temperature roasting, the diameter of sheet is 200～400nm.
Sheet with making contains gallium nano-photocatalyst photocatalytic degradation methylene blue: in photocatalytic reaction device, add 300ml 1 * 10 -5The mol/L methylene blue solution adds the catalyst that 0.03g step B makes, and keeps 30min under the half-light condition; After the adsorption equilibrium, open light source, magnetic agitation; A detection is got in segmentation, and whole process reaction pressure is normal pressure, and reaction temperature is a room temperature; Behind the reaction 15min, record that the methylene blue degradation rate is 100% behind the 15min.
Light source is a CEL-LAM500 ultraviolet light long arc mercury lamp, and the mercury lamp input power is 500W, and total length is 200mm, and power supply is input as 220V 50Hz and exchanges, and other is furnished with photochemical reactor and cold-trap, and wherein the photochemical reactor model is CEPR250, and the cold-trap model is CEQW60.
Embodiment 3
A: take by weighing 13.08g ZnCl 2With 4.22g GaCl 3Be dissolved in and be made into the 100ml mixing salt solution in the deionized water; And then take by weighing 7.68g NaOH and 5.09g Na 2CO 3Be dissolved in and be made into the 100ml mixed ammonium/alkali solutions in the deionized water; Above-mentioned two kinds of mixed solutions are added drop-wise in the four-hole boiling flask of 500ml simultaneously, and in the dropping process, keeping the pH value of reaction solution in the flask is 9, and after dropwising, keeping reaction temperature is 100 ℃, and backflow crystallization 24h obtains zinc gallium hydrotalcite precursor slurry; Zinc gallium hydrotalcite precursor slurry to pH=7.5, behind the dry 36h, promptly gets zinc gallium hydrotalcite through centrifuge washing in 60 ℃ of electric heating constant temperature air dry ovens; B: the zinc gallium hydrotalcite of above-mentioned gained is put into crucible; 800 ℃ of roasting 4h in Muffle furnace, concrete scheme is: the Muffle furnace initial temperature is 25 ℃, then with the heating rate temperature programming to 800 of 5 ℃/min ℃; And then 800 ℃ of maintenance 4h, naturally cool to room temperature afterwards; After roasting finishes, the sheet that makes is contained the gallium nano-photocatalyst take out, put into drier and preserve.
The chemical general formula of the described zinc gallium of steps A hydrotalcite precursor is:
[Zn 1-xGa x(OH) 2] X+(CO 3) 2- X/2NH 2O, wherein, x=0.2; N is the quantity of the crystallization water, n=1.9.
It is ZnO and ZnGa that the sheet that step B makes contains the gallium nano-photocatalyst 2O 4Compound, with still keeping laminated structure after its high-temperature roasting, the diameter of sheet is 200～400nm.
Sheet with making contains gallium nano-photocatalyst photocatalytic degradation methylene blue: in photocatalytic reaction device, add 300ml 1 * 10 -5The mol/L methylene blue solution adds the catalyst that 0.03g step B makes, and keeps 30min under the half-light condition; After the adsorption equilibrium, open light source, magnetic agitation; A detection is got in segmentation, and whole process reaction pressure is normal pressure, and reaction temperature is a room temperature; Behind the reaction 15min, record that the methylene blue degradation rate is 90% behind the 15min.
Light source is a CEL-LAM500 ultraviolet light long arc mercury lamp, and the mercury lamp input power is 500W, and total length is 200mm, and power supply is input as 220V 50Hz and exchanges, and other is furnished with photochemical reactor and cold-trap, and wherein the photochemical reactor model is CEPR250, and the cold-trap model is CEQW60.

Claims (6)

1. a sheet contains the preparation method of gallium nano-photocatalyst, it is characterized in that its concrete preparation process is following:
A, preparation zinc gallium hydrotalcite: take by weighing ZnCl 2And GaCl 3Be dissolved in and be made into mixing salt solution, wherein Zn in the deionized water 2+Concentration is 0.12 ~ 6mol/L, Zn 2+With Ga 3+Mol ratio is 2 ~ 4; And then take by weighing NaOH and Na 2CO 3Be dissolved in and be made into mixed ammonium/alkali solutions in the deionized water, wherein n (Na 2CO 3)/[n (Ga 3+)]=2.0 ~ 2.5, n (NaOH)/[n (Zn 2+)+n (Ga 3+)]=1.8 ~ 2.5, NaOH concentration is 1.0 ~ 6.0mol/L, n (NaOH), n (Zn 2+), n (Ga 3+), n (Na 2CO 3) be respectively NaOH, Zn 2+, Ga 3+, Na 2CO 3Molal quantity; Above-mentioned two kinds of mixed solutions are added drop-wise in the four-hole boiling flask simultaneously, and in the dropping process, keeping the pH value of reaction solution in the flask is 9 ~ 11, and after dropwising, keeping reaction temperature is 80 ~ 100 ℃, and backflow crystallization 12 ~ 36h obtains zinc gallium hydrotalcite precursor slurry; Zinc gallium hydrotalcite precursor slurry behind ℃ drying 24 ~ 48h of centrifuge washing to pH=7 ~ 8,60 ~ 80, promptly gets zinc gallium hydrotalcite;
B, the zinc gallium hydrotalcite that steps A is obtained are put into crucible; 600 ~ 900 ℃ of roasting 3 ~ 5h in Muffle furnace; Concrete scheme is: the Muffle furnace initial temperature is 15 ~ 30 ℃; Then with heating rate temperature programming to 700 ~ 900 of 5 ~ 10 ℃/min ℃, and then keep 3 ~ 5h, naturally cool to room temperature afterwards; After roasting finishes, the sheet that makes is contained the gallium nano-photocatalyst take out, put into drier and preserve.
2. a kind of sheet according to claim 1 contains the preparation method of gallium nano-photocatalyst, it is characterized in that, the chemical general formula of the described zinc gallium of steps A hydrotalcite precursor is:
[Zn 1-xGa x(OH) 2] X+(CO 3) 2- X/2NH 2O, wherein, 0.2＜x＜0.33; N is the quantity of the crystallization water, 0.1＜n＜10.
3. a kind of sheet according to claim 1 contains the preparation method of gallium nano-photocatalyst, it is characterized in that, it is ZnO and ZnGa that the described sheet of step B contains the gallium nano-photocatalyst 2O 4Compound, with still keeping laminated structure after its high-temperature roasting, the diameter of sheet is 200 ~ 400nm.
4. the sheet with step B preparation among each described preparation method of claim 1-3 contains the application of gallium nano-photocatalyst in the photocatalytic degradation methylene blue.
5. application according to claim 4 is characterized in that, the reaction condition of described photocatalytic degradation methylene blue is following: reaction pressure is a normal pressure, and reaction temperature is a room temperature, and the concentration of methylene blue in the aqueous solution is 1 * 10 -5~ 2 * 10 -5Mol/L; The quality that the adding sheet contains the gallium nano-photocatalyst is equivalent to 0.01 ~ 0.03% of system quality; Containing catalyst solution keeps 30 ~ 60min up to reaching the adsorption-desorption balance in advance under dark condition; Open light source, adopt magnetic stirring apparatus to stir reaction time 15 ~ 30min in the course of reaction.
6. application according to claim 5 is characterized in that, said light source is a CEL-LAM500 ultraviolet light long arc mercury lamp; The mercury lamp input power is 500W; Total length is 200mm, and power supply is input as 220V50Hz and exchanges, and other is furnished with photochemical reactor and cold-trap; Wherein the photochemical reactor model is CEPR250, and the cold-trap model is CEQW60.
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CN102515247B (en) * 2011-12-09 2014-03-26 浙江工业大学 Zinc-aluminum binary hydrotalcite and application thereof as photocatalytic material used for degrading methyl violet
CN103789834B (en) * 2012-10-26 2018-04-10 索尼公司 Micrometer/nanometer level gallic acid zinc crystal, Its Preparation Method And Use
CN103894172A (en) * 2012-12-28 2014-07-02 索尼公司 ZnGa2O4-Ga2O3 heterojunction photocatalytic material, preparation method and application of material
CN105435796B (en) * 2014-08-18 2017-08-25 中国科学院理化技术研究所 A kind of monovalence zinc doping hydrotalcite nano photochemical catalyst and its preparation method and application
CN104307502A (en) * 2014-10-26 2015-01-28 桂林理工大学 Visible light responding photocatalyst BaGa2ZnO5 and preparation method thereof
CN104289214A (en) * 2014-10-28 2015-01-21 桂林理工大学 Visible-light responsive photocatalyst Ba3Ga2Zn7O13, and preparation method thereof
CN105727925A (en) * 2016-02-04 2016-07-06 湖南理工学院 Preparation and application of porous structure ZnO/ZnGa2O4 visible-light-induced photocatalyst with high specific surface area
CN106268745A (en) * 2016-09-30 2017-01-04 陕西科技大学 A kind of solvent-thermal method prepares semiconductor light-catalyst ZnGa2o4and method

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CN1150985C (en) * 2002-09-06 2004-05-26 广东工业大学 Transition metal oxide/silicon dioxide nano composite powder body catalyst, its synthesis method and carbon nano tube prepared by using said catalyst
US7485600B2 (en) * 2004-11-17 2009-02-03 Honda Motor Co., Ltd. Catalyst for synthesis of carbon single-walled nanotubes
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