CN104383937B - A kind of solar energy photocatalytic agent and preparation method and application - Google Patents
A kind of solar energy photocatalytic agent and preparation method and application Download PDFInfo
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- CN104383937B CN104383937B CN201410758674.8A CN201410758674A CN104383937B CN 104383937 B CN104383937 B CN 104383937B CN 201410758674 A CN201410758674 A CN 201410758674A CN 104383937 B CN104383937 B CN 104383937B
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- solar energy
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- nitric acid
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
The invention discloses a kind of solar energy photocatalytic agent and preparation method and application.The inventive method is, weighs Fe (NO respectively3)3·9H2O、Na2HAsO4·7H2O is placed in different beaker, after deionized water dissolving, and is respectively charged in two separatory funnels, wherein, and Fe (NO3)3Solution separately adds suitable stabilizer OA；It is configured to the nitric acid that concentration is 0.2～0.8mol/L with concentrated nitric acid；Under conditions of room temperature magnetic agitation, by Fe (NO3)3Solution and Na2HAsO4Solution uses parallel flow precipitation reaction；The pH controlling mixture with nitric acid is 24, continues magnetic agitation 2h after titration under room temperature lucifuge simultaneously；Prepared light-yellow precipitate thing is washed for several times, then in drying, obtains light yellow powder product, i.e. FeAsO4Solar energy photocatalytic agent.This solar energy catalyst is applicable to degradable organic pollutant under visible light.Preparation method of the present invention is extremely simple, and mild condition is easily-controllable, beneficially large-scale promotion application.
Description
Technical field
The invention belongs to chemical and environment-friendly engineering technical field, be specifically related to a kind of solar energy photocatalytic agent
And preparation method and application.
Background technology
Photocatalitic Technique of Semiconductor can at room temperature directly utilize sunlight and be aoxidized efficiently by organic pollution
Degraded.Therefore, by photocatalysis method, make full use of sunlight carrying out degradable organic pollutant is to solve at present
One beneficial way of problem of environmental pollution.About the 4% of sunlight gross energy is only accounted for because of ultraviolet light, and can
See that light then accounts for about the 46% of sunlight gross energy, so utilizing it is critical only that of solar energy to utilize in sunlight
Visible ray.Thus, it can be seen that photocatalyst has important application prospect in current field of environmental improvement.
Summary of the invention
An object of the present invention is to provide a kind of novel solar energy photocatalytic agent, this solar energy photocatalytic
The molecular formula of agent is FeAsO4, for powder, apparent for light yellow, microstructure is irregular particle shape.
Concrete, its microstructure is the irregular particle shape of 1～15 μm.
The two of the purpose of the present invention are to provide the preparation method of a kind of above-mentioned solar energy photocatalytic agent, and it includes
Following steps in sequence:
(1) Fe (NO is weighed respectively3)3·9H2O、Na2HAsO4·7H2O is placed in different beaker, spend from
Sub-water dissolution is configured to the Fe (NO that concentration is 0.1～0.4mol/L3)3Solution and concentration are 0.1～0.4mol/L
Na2HAsO4After solution, and it is respectively charged in two separatory funnels, wherein, Fe (NO3)3In solution separately
Add suitable stabilizer OA；It is configured to the nitric acid that concentration is 0.2～0.8mol/L with concentrated nitric acid；
(2) under conditions of room temperature magnetic agitation, the Fe (NO that step (1) is prepared3)3Solution and
Na2HAsO4Solution uses parallel flow precipitation reaction；Its speed is 2～3d/s, simultaneously by step in titration process
Suddenly it is 2-4 that the nitric acid that (1) is prepared controls the pH of mixture, simultaneously after titration under room temperature lucifuge
Continue magnetic agitation 2h；
(3) the light-yellow precipitate thing that step (2) prepares is washed for several times, then dries at a temperature of 60 DEG C,
Obtain light yellow powder product, i.e. FeAsO4Solar energy photocatalytic agent.
Concrete, in step (2), during mixture reaction, control iron nitrate solution, arsenic acid hydrogen two
Sodium solution, nitric acid substance withdrawl syndrome than for 1:1:2.
The three of the purpose of the present invention are to provide the application of above-mentioned solar energy photocatalytic agent, and this solar energy is catalyzed
Agent is applicable to degradable organic pollutant under visible light.
The present invention, by a kind of method of simplicity, prepares a kind of novel solar energy photocatalytic agent FeAsO4。
By experiment, characterize FeAsO4Absorption band edge at about 650nm, the therefore utilization ratio to visible ray
High.Further, in the degraded of rhodamine B, there is obvious catalytic action.Therefore, the FeAsO of the present invention4
It it is a kind of solar energy photocatalytic agent novel, effective.Document, patent finding show, the present invention is
FeAsO4The first report of solar energy photocatalytic agent, this catalyst has potential in Organic Waste Water Treatment field
Application prospect.
The beneficial effects of the present invention is:
(1) present invention uses Na2HAsO4Preparation FeAsO4, use nitric acid to control reaction system Acidity of Aikalinity
Fe is controlled with stabilizer (OA)3+Stability, it is ensured that FeAsO4Solar energy photocatalytic characteristic.
(2) present invention is by FeAsO4Materials application in photocatalysis field, FeAsO under visible light4Have
Good rhodamine B photocatalytic activity.
(3) preparation method of the present invention is extremely simple, mild condition easily-controllable (under normal temperature and pressure, < the room of 30 DEG C
Temperature), beneficially large-scale promotion application.
Accompanying drawing explanation
Fig. 1 is FeAsO prepared by the inventive method4Scanning electron microscope (SEM) figure of photocatalyst.
Fig. 2 is FeAsO prepared by the inventive method4The X-ray diffraction (XRD) of solar energy photocatalytic agent
Figure.
Fig. 3 is FeAsO prepared by the inventive method4The ultraviolet-visible of solar energy photocatalytic agent diffuses
Spectrum (UV-Vis DRS) figure.
Fig. 4 is FeAsO prepared by the inventive method4The Activity Results figure of solar energy photocatalytic agent；Wherein,
C0The initial concentration of rhodamine B before adding for photocatalyst, i.e. 4mg/L, C are arbitrary in photocatalytic process
Time inscribe the concentration of rhodamine B.
Detailed description of the invention
The present invention is described in further detail with embodiment below in conjunction with the accompanying drawings.
Embodiment 1:
Weigh Fe (NO respectively3)3·9H2O、Na2HAsO4·7H2O is placed in different beaker, uses deionized water
Dissolve and be configured to the Fe (NO that concentration is 0.1mol/L3)3(separately adding suitable stabilizer OA) solution and concentration are
The Na of 0.1mol/L2HAsO4After solution, and it is respectively charged in two separatory funnels；It is configured to concentrated nitric acid
Concentration is the nitric acid of 0.2mol/L；Under conditions of room temperature magnetic agitation, employing parallel flow precipitation will
Fe(NO3)3Solution and Na2HAsO4Solution reaction produces the light-yellow precipitate thing with visible light catalysis activity
FeAsO4；Its speed is 2～3d/s, controls the pH of mixture in titration process with the nitric acid prepared simultaneously
It is 2～4, under room temperature lucifuge, after titration, continues magnetic agitation 2h.Nitre is controlled during mixture reaction
Acid ferrous solution, disodium hydrogen arsenate solution, nitric acid substance withdrawl syndrome ratio for 1:1:2.By light yellow
Precipitate is washed with deionized 3 times, then just obtains FeAsO in 60 DEG C of drying4Solar energy photocatalytic agent,
For buff powder.
Embodiment 2:
Weigh Fe (NO respectively3)3·9H2O、Na2HAsO4·7H2O is placed in different beaker, uses deionized water
Dissolve and be configured to the Fe (NO that concentration is 0.2mol/L3)3(separately adding suitable stabilizer OA) solution and concentration are
The Na of 0.2mol/L2HAsO4After solution, and it is respectively charged in two separatory funnels；It is configured to concentrated nitric acid
Concentration is the nitric acid of 0.4mol/L；Under conditions of room temperature magnetic agitation, employing parallel flow precipitation will
Fe(NO3)3Solution and Na2HAsO4Solution reaction produces the light-yellow precipitate thing with visible light catalysis activity
FeAsO4；Its speed is 2～3d/s, controls the pH of mixture in titration process with the nitric acid prepared simultaneously
It is 2～4, under room temperature lucifuge, after titration, continues magnetic agitation 2h.Nitre is controlled during mixture reaction
Acid ferrous solution, disodium hydrogen arsenate solution, nitric acid substance withdrawl syndrome ratio for 1:1:2.By light yellow
Precipitate is washed with deionized 3 times, then just obtains FeAsO in 60 DEG C of drying4Solar energy photocatalytic agent,
For buff powder.
Embodiment 3:
Weigh Fe (NO respectively3)3·9H2O、Na2HAsO4·7H2O is placed in different beaker, uses deionized water
Dissolve and be configured to the Fe (NO that concentration is 0.4mol/L3)3(separately adding suitable stabilizer OA) solution and concentration are
The Na of 0.4mol/L2HAsO4After solution, and it is respectively charged in two separatory funnels；It is configured to concentrated nitric acid
Concentration is the nitric acid of 0.8mol/L；Under conditions of room temperature magnetic agitation, employing parallel flow precipitation will
Fe(NO3)3Solution and Na2HAsO4Solution reaction produces the light-yellow precipitate thing with visible light catalysis activity
FeAsO4；Its speed is 2～3d/s, controls the pH of mixture in titration process with the nitric acid prepared simultaneously
It is 2～4, under room temperature lucifuge, after titration, continues magnetic agitation 2h.Nitre is controlled during mixture reaction
Acid ferrous solution, disodium hydrogen arsenate solution, nitric acid substance withdrawl syndrome ratio for 1:1:2.By light yellow
Precipitate is washed with deionized 3 times, then just obtains FeAsO in 60 DEG C of drying4Solar energy photocatalytic agent,
For buff powder.
FeAsO prepared by the present embodiment4X-ray diffraction (XRD) figure of material is as it is shown in figure 1, sample
FeAsO4Diffraction maximum and FeAsO4Standard diagram (JCPDS No.21-0910) consistent.Preparation
FeAsO4Scanning electron microscope (SEM) figure such as Fig. 2 of material.Its microstructure is very irregular as seen from the figure
Graininess, size is about 1-15 μm.FeAsO prepared by the present embodiment4The ultraviolet-visible of material is unrestrained anti-
Penetrate spectrum (Uv-Vis DRS) figure as it is shown on figure 3, sample has obvious absworption peak, energy in visible region
Absorb the visible ray less than 650nm.
FeAsO prepared by the inventive method4The visible light catalytic performance evaluation of material is as follows:
FeAsO prepared by the inventive method4The photocatalysis performance of material is by under simulated visible light, uses
The organic situation of sample degradation is evaluated, and photocatalysis experiment (includes Xe lamp at light reaction device
300W, optical filter, magnetic stirring apparatus) in carry out.Weigh sample prepared by 0.1g, add liquid dyes
In solution (4mg/L RhB) 100mL, magnetic agitation 1h under the conditions of lucifuge, reach absorption-desorption balance.
300W Xe lamp adds optical filter (λ > 420nm) as analog light source, takes 2.5mL at regular intervals and hangs
Supernatant is taken after supernatant liquid, and centrifugation (6000rpm, 5min).Use UV-2550 to supernatant
Absorbance be measured.Fig. 4 show FeAsO prepared by the inventive method4Solar energy photocatalytic agent exists
The degradation curve of catalytic degradation rhodamine B under visible light conditions, from fig. 4, it can be seen that under visible light illumination,
FeAsO prepared by the present invention4The degradable rhodamine B of photocatalyst needs 140min.
Claims (3)
1. a preparation method for solar energy photocatalytic agent, this solar energy photocatalytic agent, its molecular formula is
FeAsO4, for powder, apparent for light yellow, its microstructure is the irregular particle shape of 1～15 μm；
It is characterized in that including following steps in sequence:
(1) Fe (NO is weighed respectively3)3·9H2O、Na2HAsO4·7H2O is placed in different beaker, spend from
Sub-water dissolution is configured to the Fe (NO that concentration is 0.1～0.4mol/L3)3Solution and concentration are 0.1～0.4mol/L
Na2HAsO4After solution, and it is respectively charged in two separatory funnels, wherein, Fe (NO3)3In solution separately
Add suitable stabilizer OA；It is configured to the nitric acid that concentration is 0.2～0.8mol/L with concentrated nitric acid；
(2) under conditions of room temperature magnetic agitation, the Fe (NO that step (1) is prepared3)3Solution and
Na2HAsO4Solution uses parallel flow precipitation reaction；Its speed is 2～3d/s, simultaneously by step in titration process
Suddenly it is 2-4 that the nitric acid that (1) is prepared controls the pH of mixture, simultaneously after titration under room temperature lucifuge
Continue magnetic agitation 2h；
(3) the light-yellow precipitate thing that step (2) prepares is washed for several times, then dries at a temperature of 60 DEG C,
Obtain light yellow powder product, i.e. FeAsO4Solar energy photocatalytic agent.
The preparation method of solar energy photocatalytic agent the most according to claim 1, it is characterised in that: step
(2), in, iron nitrate solution, disodium hydrogen arsenate solution, the thing of nitric acid during mixture reaction, are controlled
The amount concentration of matter is than for 1:1:2.
3. the solar energy that prepared by the preparation method of a solar energy photocatalytic agent as claimed in claim 1
The application of catalyst, it is characterised in that: it is applicable to degradable organic pollutant under visible light.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008013124A1 (en) * | 2006-07-27 | 2008-01-31 | Dowa Metals & Mining Co., Ltd. | Iron arsenate powder |
| CN101274774A (en) * | 2008-05-16 | 2008-10-01 | 株洲市众乐化工有限责任公司 | Arsenic-removing method for producing nanometer- zinc oxide by ammonia leaching method |
| JP2008260683A (en) * | 2006-04-28 | 2008-10-30 | Dowa Metals & Mining Co Ltd | Iron arsenate powder |
| CN103071496A (en) * | 2013-02-05 | 2013-05-01 | 湖南科技大学 | Visible-light-driven photocatalyst and preparation method and application thereof |
| CN103418316A (en) * | 2010-01-29 | 2013-12-04 | 张颖 | Preparation method of modified micro-granules |
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2014
- 2014-12-11 CN CN201410758674.8A patent/CN104383937B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008260683A (en) * | 2006-04-28 | 2008-10-30 | Dowa Metals & Mining Co Ltd | Iron arsenate powder |
| WO2008013124A1 (en) * | 2006-07-27 | 2008-01-31 | Dowa Metals & Mining Co., Ltd. | Iron arsenate powder |
| CN101495412A (en) * | 2006-07-27 | 2009-07-29 | 同和金属矿业有限公司 | Iron arsenate powder |
| CN101274774A (en) * | 2008-05-16 | 2008-10-01 | 株洲市众乐化工有限责任公司 | Arsenic-removing method for producing nanometer- zinc oxide by ammonia leaching method |
| CN103418316A (en) * | 2010-01-29 | 2013-12-04 | 张颖 | Preparation method of modified micro-granules |
| CN103071496A (en) * | 2013-02-05 | 2013-05-01 | 湖南科技大学 | Visible-light-driven photocatalyst and preparation method and application thereof |
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