CN108295883A - A kind of Ag3PO4The preparation and application of/CNH photocatalysis nano materials - Google Patents
A kind of Ag3PO4The preparation and application of/CNH photocatalysis nano materials Download PDFInfo
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- SRUWWOSWHXIIIA-UKPGNTDSSA-N Cyanoginosin Chemical compound N1C(=O)[C@H](CCCN=C(N)N)NC(=O)[C@@H](C)[C@H](C(O)=O)NC(=O)[C@H](CC(C)C)NC(=O)[C@H](C)NC(=O)C(=C)N(C)C(=O)CC[C@H](C(O)=O)N(C)C(=O)[C@@H](C)[C@@H]1\C=C\C(\C)=C\[C@H](C)[C@@H](O)CC1=CC=CC=C1 SRUWWOSWHXIIIA-UKPGNTDSSA-N 0.000 abstract description 20
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Classifications
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- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- 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
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Health & Medical Sciences (AREA)
- Toxicology (AREA)
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Abstract
The invention belongs to photocatalytic environmental-protection fields, and in particular to a kind of Ag of catalytic degradation Microcystin3PO4The preparation method of/CNH composite photocatalyst nano materials and application.The technology of photocatalytic degradation Microcystin of the present invention is compared to traditional treatment process, with non-secondary pollution, the advantages that safety and stability, cost is relatively low, to there is significant degradation effect with the toxic organic pollutant that Microcystin (MC) is representative.The present invention uses nitric acid hydro-thermal process method, prepares the g C of protonation3N4Nano material, this preparation method have the characteristics that simple and do not generate impurity.Then by chemical precipitation method successfully synthesize different quality than Ag3PO4/ CNH composite materials are formed on its surface hetero-junctions and utilize photocatalytic degradation MC.Prepared composite photocatalyst material may be used on the field of eutrophied water treatment, have good practical value and application prospect.
Description
Technical field：
The invention belongs to photocatalytic environmental-protection fields, and in particular to a kind of Ag of catalytic degradation Microcystin3PO4/ CNH is multiple
Close the preparation and application of visible light catalytic nano material.
Background technology：
Eutrophication is environmental problem universal in global range, with the development of society, a large amount of industrial wastewater and
Sanitary sewage is discharged into water body and the dynamics of aquaculture and intensity constantly expand, and natural water eutrophication is caused to add
Speed has directly facilitated the generation of wawter bloom in rivers and lakes.Cyanobacteria be it is a kind of it is extensive growth and the harmful algae in water body that swims,
Microcystin (MC) is frequency of occurrences highest, one kind of yield maximum and the most serious that causes damages that the malicious cyanobacteria of production releases
Algae toxin threatens aquatic animal and the health of the mankind.So far, it was found that nearly 90 various microcystins.Therefore micro-capsule
The pollution problem of algae toxin causes the attention of numerous researchers and relevant department and has carried out a series of research to it.
Microcystin has the chemical property of quite stable, therefore general water treatment technology is difficult thoroughly to go it
It removes.Studies have found that after Adda structures in visible photo damage Microcystin, the toxicity of algae toxin significantly reduces, however
Visible light accounts for about the 43% of solar energy in natural light.Therefore, it is seen that the photocatalysis of light has huge potentiality as renewable
With sustainable method for treating water.
Class graphite phase carbon nitride (g-C3N4) as a kind of novel, to being responded under visible light nonmetallic materials, due to it
The advantages that chemical stability is good, energy gap is relatively narrow, preparation method is easy is widely paid close attention to.But at this stage, due to g-C3N4
, hydrophobicity strong, electron-hole recombination rate high the shortcomings of small by specific surface area, is limited, its practical application is hindered.Although people
Can improve g-C by template and non-template method3N4Specific surface area, but there are synthesis cost height and easily cause two to template
The shortcomings of secondary pollution；And the non-templates rule such as soda acid etching exists to g-C3N4Specific surface area increase rate it is relatively low the deficiencies of it
Place.The main research and utilization nitric acid hydro-thermal process method of the present invention, prepares the g-C of protonation3N4Nano material, this preparation method have
The characteristics of simply and not generating impurity.G-C after Nitric acid etching3N4, larger specific surface area can be obtained, band gap is wide
Degree is reduced significantly, and has stronger photocatalytic activity and stability.Here by the g-C of protonation3N4It is named as CNH.Then pass through
Chemical precipitation method successfully synthesize different quality than Ag3PO4/ CNH composite materials are formed on its surface hetero-junctions and utilize light
Catalytic degradation MC, to the catalytic activity of the synthesized material of assessment.
Invention content：
The purpose of the present invention is to provide a kind of Ag of catalytic degradation MC3PO4The preparation side of/CNH composite photocatalyst materials
Method.Obtained photochemical catalyst is conducive to the transmission process of photo-generated carrier, has good visible light photocatalysis active.
It is a further object of the present invention to provide Ag3PO4The application of/CNH visible light catalysts.
In order to realize first above-mentioned purpose, present invention employs technical solutions below：
A kind of Ag3PO4/ CNH composite visible light responsible photocatalytic materials, are by Ag3PO4With the composite photocatalyst of CNH compositions
Material, Ag in composite catalyzing material3PO4Mass ratio be 10wt%, 20wt% and 30wt%.
1, a kind of Ag3PO4The preparation method of/CNH composite visible light catalytic materials, includes the following steps：
(1) 30g melamines are positioned in the alumina crucible of 100mL, then crucible is positioned in Muffle furnace and is forged
It burns, obtains yellow powder, as g-C3N4；
(2) g-C of gained in step (1) is taken3N4Powder is added to HNO3In solution, magnetic agitation keeps powder evenly dispersed
In the solution；
(3) solution described in step (2) is transferred in autoclave and is reacted, then cooled to room temperature, centrifugation point
From taking-up sediment absolute ethyl alcohol and milli-Q water.It is finally positioned over drying in vacuum drying chamber, obtains the g- of acid etch
C3N4, as CNH；
(4) by AgNO3It is dissolved in the ultra-pure water of 100mL.The CNH powder that 1g has been prepared is weighed, above-mentioned solution is put into
Middle ultrasound keeps powder evenly dispersed in the solution；
(5) 0.33g Na are weighed3PO4·12H2O is dissolved in 100mL ultra-pure waters, then by Na3PO4Solution is slowly dropped into
AgNO3With CNH mixed liquors, Ag is avoided3PO4Photodissociation, centrifuge, take out sediment；
(6) sediment 3 times in step (5) are respectively washed with absolute ethyl alcohol and ultra-pure water.It is finally positioned in vacuum drying chamber and does
It is dry.Finally, Ag is made3PO4/ CNH catalysis materials.
2, in the above method, step (1) described Muffle furnace is warming up to 550 DEG C with the heating rate of 2.5 DEG C/min, keeps forging
Burn 4h.It takes out sample and is cooled to room temperature, ground sample obtains g-C3N4Powder.
3, in the above method, step (2) described solution is the 0.5M HNO of 40mL3In solution, the magnetic agitation time is
30min。
4, in the above method, the reaction temperature of step (3) described autoclave is 160 DEG C, reaction time 7h, precipitation
Object absolute ethyl alcohol and ultra-pure water are respectively washed 3 times.
5, in the above method, the temperature of step (3) vacuum drying chamber is drying time 12h in 80 DEG C.
6, in the above method, the ultrasonic time of step (4) is 0.5h.
7, in the above method, the reaction condition of step (5) solution is to be protected from light magnetic agitation 4h.
8, in the above method, the temperature of step (6) vacuum drying chamber is drying time 12h in 80 DEG C.
In order to realize another above-mentioned purpose, present invention employs technical solutions below：
A kind of Ag3PO4/ CNH composite photocatalyst materials photocatalytic degradation Microcystin (MC) under visible light conditions are answered
With.
Compared with prior art, the invention has the advantages that：
(1) preparation method of the invention have simple for process, mild condition, stability it is good, it is of low cost, can efficiently utilize
A kind of monomer need to only be mixed with another monomer, composite wood generated by simple chemical precipitation method by the advantages that solar energy
Material；
(2) composite photocatalyst material prepared by preparation method through the invention is laminated structure, has larger ratio table
Area is conducive to the fast transferring of photo-generated carrier, to have high photocatalytic activity, compared with CNH, Ag3PO4/ CNH is multiple
Closing light catalysis material further improves the response to visible light, has higher removal efficiency；
(3) under the irradiation of 350W xenon lamps, which shows good degradation effect to MC, using too
It is positive to be had potential application in photocatalysis Decomposition toxic organic pollutant treatment technology.
Description of the drawings
Fig. 1 is Ag of the present invention3PO4The field emission scanning electron microscope figure (FESEM) of/CNH composite visible light catalytic materials.
Fig. 2 is CNH and Ag of the present invention3PO4The XRD spectrum of/CNH composite photocatalyst materials
Fig. 3 is the pure g-C of the present invention3N4, CNH and Ag3PO4/ CNH composite visible light catalytic materials are to Microcystin (MC)
Light degradation design sketch.
Specific implementation mode
The following describes the present invention in detail with reference to examples, so that those skilled in the art more fully understand this hair
It is bright, but the invention is not limited in following embodiments.
Embodiment 1：
The preparation of CNH：30g melamines are positioned in the alumina crucible of half point closed state of 100mL, then
Crucible is positioned in Muffle furnace, and 550 DEG C are warming up to the heating rate of 2.5 DEG C/min, keeps calcining 4h.Sample is taken out to be cooled to
Room temperature, ground sample, finally obtained product are g-C3N4Powder.
Embodiment 2：
Take the g-C that 1g is prepared3N4Powder is added to the 0.5M HNO of 40mL3In solution, magnetic agitation 30min makes powder
It is evenly dispersed that suspension is transferred in autoclave in the solution, 7h is reacted at 160 DEG C, is then cooled to room temperature, from
The heart detaches, and takes out sediment, is respectively washed 3 times with absolute ethyl alcohol and ultra-pure water.It is finally positioned over vacuum drying chamber, it is dry in 80 DEG C
12h is to get CNH.
Embodiment 3：
Ag3PO4The preparation of/CNH composite photocatalyst materials：Take 0.1g AgNO3It is dissolved in the ultra-pure water of 100mL.It weighs
The CNH powder that 1g has been prepared, is put into above-mentioned solution, and ultrasound 0.5h, keeps powder evenly dispersed in the solution.It weighs
0.33g Na3PO4·12H2O is dissolved in 100mL ultra-pure waters, then by Na3PO4Solution is slowly dropped into AgNO3With CNH mixed liquors
In, it is protected from light magnetic agitation 4h, avoids Ag3PO4Photodissociation, centrifuge, take out sediment, respectively wash 3 with absolute ethyl alcohol and ultra-pure water
It is secondary.It is finally positioned over vacuum drying chamber, the dry 12h in 80 DEG C.Ag is made3PO4/ CNH catalysis materials, wherein Ag3PO4
Mass ratio in composite photocatalyst material is 10wt%.
Ag3PO4The sem analysis result (Fig. 1) of/CNH composite photocatalyst materials shows figure Ag3PO4Disperse in nanoparticulate
On the surface of CNH.In the composite, Ag3PO4Interaction between CNH materials makes Ag3PO4Nano-particle is averaged
Size reduces, and prevents Ag to a certain extent3PO4The reunion of particle.Ag3PO4Good dispersibility makes photocatalysis material
The specific surface area of material obviously increases, and the efficiency for being conducive to composite material light-catalyzed reaction improves.
The XRD analysis result of different catalysis materials is shown in Fig. 2, passes through the Ag of CNH and different composite ratio3PO4/ CNH photocatalysis
Material comparison finds Ag3PO4Each diffraction maximum and card (JCPDS：Corresponding diffraction maximum position is one by one in 06-0505)
It is corresponding.Illustrate Ag3PO4CNH lattices are not entered into, the variation of CNH internal structures is not caused, and are only attached to its surface, with
Ag3PO4The peak intensity of the reduction of content, CNH is also weakened.Simultaneously in Ag3PO4/ CNH composite photocatalyst material XRD spectras
In, there is no the appearance of the diffraction maximum of other materials, illustrate Ag3PO4, CNH combination do not generate other new substances.
The pure g-C prepared3N4, CNH and Ag3PO4/ CNH composite visible light catalytic materials in 2h to Microcystin can
Light-exposed degradation rate result is shown in Fig. 3.
Embodiment 4：
Except for the following differences, remaining is the same as embodiment 3 for operating process.
Weigh 0.2g AgNO3With the CNH powder of gained in 1g embodiments 2, wherein Ag3PO4In composite photocatalyst material
Mass ratio be 20wt%.
The XRD analysis result of sample is shown in Fig. 2.The sem analysis result of sample is similar to Example 3.Sample is in 2h to micro-
The Visible Light Induced Photocatalytic rate result of capsule algae toxin is shown in Fig. 3.
Embodiment 5：
Except for the following differences, remaining is the same as embodiment 4 for operating process.
Weigh 0.3g AgNO3With the CNH powder of gained in 1g embodiments 2, wherein Ag3PO4In composite photocatalyst material
Mass ratio be 30wt%.
The XRD analysis result of sample is shown in Fig. 2.The sem analysis result of sample is similar to Example 3.Sample is in 2h to micro-
The Visible Light Induced Photocatalytic rate result of capsule algae toxin is shown in Fig. 3.
Embodiment 6：
Photocatalytic activity evaluation：In visible light photocatalytic degradation device (the XPA series photochemical reactions of 26 DEG C of a constant temperature
Instrument, Xujiang Electromechanical Plant, Nanjing, China) in carry out, light source is 350W xenon lamps, and visible light is obtained by loading optical filter (420nm).It will
MC (15mg/L) solution of 10mL is placed in quartz glass tube and g-C is added3N4Photochemical catalyst 0.05g is then placed in photocatalysis instrument
In device reactor, in order to exclude the influence of physisorption, reaction first carries out the dark absorption of 60min, makes catalysis before starting
Simultaneously adsorption equilibrium is contacted between agent and Microcystin molecule enough.Reach reaction adsorption equilibrium after open xenon source, into
Stirring instrument is opened when row secretly adsorbs, the purpose of stirring is to maintain catalyst and is in suspension or afloat, and it is uniform to be allowed to receiving
Illumination.During Xenon light shining 1mL, sustained response 120min are sampled at interval of 30min.The Sample storage taken out 10mL from
It in heart pipe, and places in the dark, is separated water sample and catalyst using centrifuge, preserve supernatant and wait for detection and analysis.
The experimental results showed that within the reaction time of 2h, with the increase in reaction time, degradation efficiency improves, wherein g-
C3N4It is 11.3% to the degradation rate of Microcystin in Xenon light shining 2h.
Embodiment 7：
Except for the following differences, remaining is the same as embodiment 6 for operating process.
CNH photochemical catalysts 0.05g is added.
The experimental results showed that within the reaction time of 2h, with the increase in reaction time, degradation efficiency improves, wherein
CNH is 14.7% to the degradation rate of Microcystin in Xenon light shining 2h.
Embodiment 8：
Except for the following differences, remaining is the same as embodiment 7 for operating process.
CNH and Ag is added3PO4/ CNH composite photocatalyst materials 0.05g.
The experimental results showed that within the reaction time of 2h, with the increase in reaction time, degradation efficiency improves, wherein when
Ag3PO4When mass ratio in composite photocatalyst material is 20wt%, composite material visible light photocatalytic degradation MC has best
Effect, the degradation rate in Xenon light shining 2h is up to 79.8%, compared to pure g-C3N4Have significantly with the degradation effect of CNH
It improves, 7.06 times and 5.43 times have been respectively increased in degradation effect.
The embodiment is the preferred embodiments of the present invention, but present invention is not limited to the embodiments described above, not
Away from the present invention substantive content in the case of, those skilled in the art can make it is any it is conspicuously improved, replace
Or modification all belongs to the scope of protection of the present invention.
Claims (9)
1. a kind of Ag3PO4The preparation method of/CNH photocatalysis nano materials, which is characterized in that include the following steps：
(1) 30g melamines are positioned in the alumina crucible of 100mL, then crucible is positioned in Muffle furnace and is calcined, is obtained
To yellow powder, as g-C3N4；
(2) g-C of gained in step (1) is taken3N4Powder is added to HNO3In solution, it is molten that magnetic agitation makes powder be dispersed in
In liquid；
(3) solution described in step (2) is transferred in autoclave and is reacted, then cooled to room temperature, centrifuged, take
Go out sediment absolute ethyl alcohol and milli-Q water, is finally positioned over drying in vacuum drying chamber, obtains the g-C of acid etch3N4, i.e.,
For CNH；
(4) by AgNO3It is dissolved in the ultra-pure water of 100mL, weighs the CNH powder that 1g has been prepared, be put into above-mentioned solution and surpass
Sound keeps powder evenly dispersed in the solution；
(5) 0.33g Na are weighed3PO4·12H2O is dissolved in 100mL ultra-pure waters, then by Na3PO4Solution is slowly dropped into AgNO3
With CNH mixed liquors, Ag is avoided3PO4Photodissociation, centrifuge, take out sediment；
(6) sediment 3 times in step (5) are respectively washed with absolute ethyl alcohol and ultra-pure water, is finally positioned in vacuum drying chamber dry, system
Obtain Ag3PO4/ CNH catalysis materials.
2. Ag according to claim 13PO4The preparation method of/CNH composite visible light catalytic materials, which is characterized in that step
Suddenly (1) described Muffle furnace is warming up to 550 DEG C with the heating rate of 2.5 DEG C/min, keeps calcining 4h, takes out sample and is cooled to often
Temperature, ground sample obtain g-C3N4Powder.
3. Ag according to claim 13PO4The preparation method of/CNH composite visible light catalytic materials, which is characterized in that step
Suddenly (2) described solution is the 0.5M HNO of 40mL3In solution, the magnetic agitation time is 30min.
4. Ag according to claim 13PO4The preparation method of/CNH composite visible light catalytic materials, which is characterized in that step
Suddenly the reaction temperature of (3) described autoclave is 160 DEG C, reaction time 7h, and sediment absolute ethyl alcohol and ultra-pure water are each
It washes 3 times.
5. Ag according to claim 13PO4The preparation method of/CNH composite visible light catalytic materials, which is characterized in that step
Suddenly the temperature of (4) vacuum drying chamber is drying time 12h in 80 DEG C.
6. Ag according to claim 13PO4The preparation method of/CNH composite visible light catalytic materials, which is characterized in that step
Suddenly the ultrasonic time of (5) is 0.5h.
7. Ag according to claim 13PO4The preparation method of/CNH composite visible light catalytic materials, which is characterized in that step
Suddenly the reaction condition of (6) solution is to be protected from light magnetic agitation 4h.
8. Ag according to claim 13PO4The preparation method of/CNH composite visible light catalytic materials, which is characterized in that step
Suddenly the temperature of (7) vacuum drying chamber is drying time 12h in 80 DEG C.
9. a kind of Ag being prepared according to claim 13PO4The application of/CNH composite photocatalyst materials, which is characterized in that institute
State application of the catalysis material in degrading microcystic toxins.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109876842A (en) * | 2019-01-26 | 2019-06-14 | 华南理工大学 | A kind of g-C3N4/Fe/Ag3PO4Composite material and preparation method and application |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103028428A (en) * | 2013-01-16 | 2013-04-10 | 华东理工大学 | Method for preparing composite visual light catalytic material Ag3PO4 and g-C3N4 |
| CN103464191A (en) * | 2013-09-29 | 2013-12-25 | 天津工业大学 | Graphite type carbon nitride and silver phosphate compound photocatalytic materials and preparation method thereof |
| CN103506141A (en) * | 2013-09-29 | 2014-01-15 | 太原理工大学 | Method for preparing visible light photocatalytic material and application thereof |
| JP2014177378A (en) * | 2013-03-14 | 2014-09-25 | Nissan Chem Ind Ltd | Method for producing porous carbon nitride |
-
2018
- 2018-02-02 CN CN201810105813.5A patent/CN108295883A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103028428A (en) * | 2013-01-16 | 2013-04-10 | 华东理工大学 | Method for preparing composite visual light catalytic material Ag3PO4 and g-C3N4 |
| JP2014177378A (en) * | 2013-03-14 | 2014-09-25 | Nissan Chem Ind Ltd | Method for producing porous carbon nitride |
| CN103464191A (en) * | 2013-09-29 | 2013-12-25 | 天津工业大学 | Graphite type carbon nitride and silver phosphate compound photocatalytic materials and preparation method thereof |
| CN103506141A (en) * | 2013-09-29 | 2014-01-15 | 太原理工大学 | Method for preparing visible light photocatalytic material and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| YONGCAI ZHANG ET AL.,: ""Acid-treated g-C3N4 with improved photocatalytic performance in the reduction of aqueous Cr(VI) under visible-light"", 《SEPARATION AND PURIFICATION TECHNOLOGY》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109876842A (en) * | 2019-01-26 | 2019-06-14 | 华南理工大学 | A kind of g-C3N4/Fe/Ag3PO4Composite material and preparation method and application |
| CN109876842B (en) * | 2019-01-26 | 2021-07-20 | 华南理工大学 | g-C3N4/Fe/Ag3PO4Composite material and preparation method and application thereof |
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