CN104722324A - Method for preparing Ag-g-C3N4/TiO2 ternary complex by three-step method - Google Patents
Method for preparing Ag-g-C3N4/TiO2 ternary complex by three-step method Download PDFInfo
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- CN104722324A CN104722324A CN201510042379.7A CN201510042379A CN104722324A CN 104722324 A CN104722324 A CN 104722324A CN 201510042379 A CN201510042379 A CN 201510042379A CN 104722324 A CN104722324 A CN 104722324A
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- tio2
- powder
- tio
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Abstract
The invention discloses a method for preparing an Ag-g-C3N4/TiO2 ternary complex by a three-step method. The method is characterized by comprising the following steps: firstly, heating a reagent (melamine) to 540 DEG C, and cracking the reagent into graphite-like carbonized nitrogen (g-C3N4); further performing ultrasonic mixing to enable P25 to load g-C3N4; and finally, doping silver with an immobilized sol process and synthesizing a target product. A composite photocatalyst with the structure has high visible-light activity so as to become an important sewage treating agent with potential research value. The method disclosed by the invention has the advantages of simple reaction condition, moderate and stable reaction and easy large-scale production.
Description
Technical field
The present invention relates to a kind of preparation method of ternary complex, particularly relate to a kind of three-step approach and produce Ag-g-C
3n
4 /tiO
2the method of ternary complex.
Background technology
Ag-g-C
3n
4 /tiO
2ternary can compound be a kind of visible-light photocatalyst, because of this Three-element composite photocatalyst tool visible light activity, thus becomes a kind of important sewage-treating agent with potential researching value.More to the research of binary composite photo-catalyst both at home and abroad, but not yet there is preparation Ag-g-C
3n
4 /tiO
2the report of Three-element composite photocatalyst.Therefore without the preparation method of complete this Three-element composite photocatalyst of synthesis; The present invention take melamine as primary raw material, successively by Pintsch process, ultrasonic mixing, immobilization colloidal sol three step process, finally obtained target product.
Summary of the invention
A kind of three-step approach is the object of the present invention is to provide to produce Ag-g-C
3n
4 /tiO
2the method of ternary complex, this preparation method take melamine as raw material, successively by Pintsch process, ultrasonic mixing, immobilization colloidal sol three step finally obtained Ag-g-C
3n
4 /tiO
2tri compound high-performance optical catalyst.
The present invention is achieved like this, and it is characterized in that preparation method is:
Step 1, melamine is loaded in porcelain crucible, is placed in Muffle furnace, slowly rises to temperature 540 by room temperature
oc, and after constant temperature 2 h, Temperature fall.Take out after being cooled to room temperature, after weighing, sample is ground into powder and obtains light yellow photochemical catalyst g-C
3n
4.
Step 2, take TiO2 solid powder, be placed in Rotary Evaporators, add ethanol solution, then add the g-C3N4 that step 1 obtains, the weight ratio 1:2-10 of TiO2 and g-C3N4.Then ultrasonic mixing 15 min disperses completely to powder.80
oc vacuum drying 5 h obtains powder, after grinder grinding, in Muffle furnace 400
o2 h are calcined under C condition.Temperature fall.Take out after being cooled to room temperature, then be ground into powder with grinder, obtain binary composite photo-catalyst g-C
3n
4 /tiO
2.
Step 3, collargol pass through NaBH
4make reducing agent oxidation AgNO
3and obtain, and make protective agent to reach good dispersiveness with polyvinyl alcohol (PVA).
Detailed process is as follows: get 8 mL AgNO
3the aqueous solution (Ag content is 1.60 mgmL
-1i.e. 12.8 mg, 0.1187 mmol Ag), mix with protective agent PVA (getting 8.5 mg PVA to be dissolved in 8.0 ml water) in ice-water bath (
m ag:
m pVA=1.5:1) and vigorous stirring, then add NaBH fast
4the aqueous solution, Ag and NaBH
4mol ratio be 1:5.NaBH
4solution: by 22.45 mg NaBH
4be dissolved in 9.60 mL water, when colloidal sol becomes black from colourless, show that silver sol is formed.In ultrasonic cavitation and under stirring, by load capacity m
ag: m
tiO2about=1.0% carrier g-C
3n
4/ TiO
2join in silver sol suspension, both maintenances contact, until all absorb, obtains target product Ag-g-C
3n
4 /tiO
2, then wet solid catalyst is placed in 80 ° of C drying boxes dry.Rearmounted drier in be cooled to room temperature, after weighing preserve, obtain Three-element composite photocatalyst Ag-g-C3N4/TiO2.
Advantage of the present invention is: employing Pintsch process melamine prepares g-C3N4, the ultrasonic g-C3N4/TiO2 of being mixed with, Ag-g-C prepared by immobilization colloidal sol
3n
4 /tiO
2, three-steps process reaction condition is simple, reaction temperature and and stable, be easy to amplify and produce.
Accompanying drawing explanation
Fig. 1 is that the UV-vis DRS of embodiment of the present invention gained sample composes.
Fig. 2 is the visible light activity of different photochemical catalyst of the present invention.
Detailed description of the invention
1. melamine pyrolysis prepares g-C
3n
4
Take 3 g melamines and be placed in 50 mL porcelain crucibles, put into Muffle furnace, rise to temperature 540 by room temperature
oc, after constant temperature 2 h, Temperature fall.Take out after being cooled to room temperature, obtain g-C
3n
4, after weighing, be ground into powder sample preservation.
2. be ultrasonicly mixed with g-C
3n
4 /tiO
2
Take 0.10 gTiO respectively
2pressed powder four parts is placed in four 100 mL beakers, respectively adds ethanol solution 50 mL, then adds the g-C of 0.002 g, 0.004 g, 0.008 g, 0.01 g respectively
3n
4powder, namely obtains g-C
3n
4 /tiO
2mass ratio is respectively: 2%, 4%, 8%, 10%.Then ultrasonic mixing 15 min disperses completely to powder.80
oc is dry, and 5 h obtain powder with evaporate to dryness, to be placed in Muffle furnace 400 after grinding
o2 h are calcined under C condition.Temperature fall.Take out after being cooled to room temperature, after having claimed, be ground into powder sample preservation.
3, fixing solation technique prepares target product Ag-g-C
3n
4 /tiO
2
Detailed process is as follows: the AgNO getting 8 mL
3(Ag content is 1.60 mgmL to the aqueous solution
-1, i.e. 12.8 mg, 0.1187 mmol Ag), mix with protective agent PVA (getting 8.6 mg PVA to be dissolved in 8.0 ml water) in ice-water bath (
m ag:
m pVA=1.5:1) and vigorous stirring, then add NaBH fast
4the aqueous solution (22.45 mg NaBH
4be dissolved in 9.60 mL water) (
n ag:
n naBH4=1:5), when colloidal sol becomes black from colourless, show that silver sol is formed.In ultrasonic cavitation and under stirring, by load capacity m
ag: m
g-C3N4/TiO2=0.5,1.0,1.5,2.0,3.0% carrier g-C
3n
4 /tiO
2join in silver sol suspension, both maintenances contact, until all absorb, obtains target product Ag-g-C
3n
4 /tiO
2.Then wet solid catalyst is placed in 80 ° of C drying boxes dry.Rearmounted drier in be cooled to room temperature, after weighing preserve.
4, photochemical catalyst characterizes and tests with photocatalysis performance
as shown in Figure 1 and Figure 2, with UV-Vis diffuse reflection spectroscopy, photochemical catalyst sample is characterized, and (it is 10 mg that 100 mg catalyst add 100 mL concentration to determine the ability of photocatalyst for degrading methylene blue (MB)
/in the MB of L, under lucifuge stirring condition, adsorb 2 h, add 420 nm optical filters afterwards, then irradiate 4 h) with 500 W xenon lamps.
Claims (1)
1. three-step approach produces Ag-g-C
3n
4 /tiO
2the method of ternary complex, is characterized in that method step is:
Step 1, melamine is loaded in porcelain crucible, is placed in Muffle furnace, slowly rises to temperature 540 by room temperature
oc, and after constant temperature 2 h, Temperature fall, takes out after being cooled to room temperature, after weighing, is ground into powder by sample and obtains light yellow photochemical catalyst g-C
3n
4;
Step 2, take TiO2 solid powder, be placed in Rotary Evaporators, add ethanol solution, then add the g-C3N4 that step 1 obtains, the weight ratio 1:2-10 of TiO2 and g-C3N4, then ultrasonic mixing 15 min disperses completely to powder, and 80
oc vacuum drying 5 h obtains powder, after grinder grinding, in Muffle furnace 400
o2 h are calcined, Temperature fall under C condition; Take out after being cooled to room temperature, then be ground into powder with grinder, obtain binary composite photo-catalyst g-C
3n
4 /tiO
2;
Step 3, collargol pass through NaBH
4make reducing agent oxidation AgNO
3and obtain, and make protective agent to reach good dispersiveness with polyvinyl alcohol;
Detailed process is as follows: get 8 mL AgNO
3the aqueous solution, wherein Ag content is 1.60 mgmL
-1, mix with protective agent PVA in ice-water bath, wherein
m ag:
m pVA=1.5:1, and vigorous stirring, then add NaBH fast
4the aqueous solution, Ag and NaBH
4mol ratio be 1:5; NaBH
4solution: by 22.45 mg NaBH
4be dissolved in 9.60 mL water, when colloidal sol becomes black from colourless, show that silver sol is formed, in ultrasonic cavitation and under stirring, by load capacity m
ag: m
tiO2about=1.0% carrier g-C
3n
4/ TiO
2join in silver sol suspension, both maintenances contact, until all absorb, obtains target product Ag-g-C
3n
4 /tiO
2, then wet solid catalyst is placed in 80 ° of C drying boxes dry, rearmounted drier in be cooled to room temperature, preserve after weighing, obtain Three-element composite photocatalyst Ag-g-C3N4/TiO2.
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Cited By (9)
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CN105148972A (en) * | 2015-09-10 | 2015-12-16 | 上海大学 | Preparation method and application of novel catalyst for reducing nitrate nitrogen in water under visible light condition |
CN105572176A (en) * | 2016-02-25 | 2016-05-11 | 济南大学 | Preparation method and application of toluene gas sensor based on non-noble metal doped composite material |
CN105665733A (en) * | 2015-11-24 | 2016-06-15 | 鲁东大学 | Method for preparing graphite-like C3N4/nano-silver antibacterial composite in environmental-friendly mode |
CN106971863A (en) * | 2017-04-21 | 2017-07-21 | 华中科技大学 | A kind of g C3N4/NiCo2S4Composite, preparation method and applications |
CN107475745A (en) * | 2017-08-23 | 2017-12-15 | 黄河科技学院 | Phosphorus doping nitridation carbon composite modified titanic oxide optoelectronic pole, its preparation method and the application of a kind of gold modification |
CN108212190A (en) * | 2017-12-29 | 2018-06-29 | 长沙理工大学 | A kind of Ag bases three-dimensional sea urchin shape E-g-C3N4/ TiO2 composite materials and preparation method thereof |
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CN113941357A (en) * | 2021-12-02 | 2022-01-18 | 塔里木大学 | Si-TiO2/g-C3N4Ternary composite photocatalytic material and preparation method thereof |
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CN101791565A (en) * | 2010-03-30 | 2010-08-04 | 湘潭大学 | TiO2@ graphite phase carbon nitride heterojunction composite photocatalyst and preparation method thereof |
CN102626650A (en) * | 2012-03-20 | 2012-08-08 | 浙江理工大学 | Preparation method of nanometer porous nitrogen doped titanium oxide visible photocatalyst |
CN103230808A (en) * | 2013-05-25 | 2013-08-07 | 南昌航空大学 | Method for preparing Pt-C3N4-TiO2 three-component visible light photocatalyst |
CN103418415A (en) * | 2013-08-22 | 2013-12-04 | 南昌航空大学 | Method for using ultrasonic mixing to prepare Ag-g-C3N4/TiO2 photocatalyst |
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CN101791565A (en) * | 2010-03-30 | 2010-08-04 | 湘潭大学 | TiO2@ graphite phase carbon nitride heterojunction composite photocatalyst and preparation method thereof |
CN102626650A (en) * | 2012-03-20 | 2012-08-08 | 浙江理工大学 | Preparation method of nanometer porous nitrogen doped titanium oxide visible photocatalyst |
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Cited By (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105148972A (en) * | 2015-09-10 | 2015-12-16 | 上海大学 | Preparation method and application of novel catalyst for reducing nitrate nitrogen in water under visible light condition |
CN105665733A (en) * | 2015-11-24 | 2016-06-15 | 鲁东大学 | Method for preparing graphite-like C3N4/nano-silver antibacterial composite in environmental-friendly mode |
CN105572176A (en) * | 2016-02-25 | 2016-05-11 | 济南大学 | Preparation method and application of toluene gas sensor based on non-noble metal doped composite material |
CN105572176B (en) * | 2016-02-25 | 2018-04-03 | 济南大学 | A kind of preparation method and application of the toluene gas sensor based on base metal doped and compounded material |
CN106971863A (en) * | 2017-04-21 | 2017-07-21 | 华中科技大学 | A kind of g C3N4/NiCo2S4Composite, preparation method and applications |
CN106971863B (en) * | 2017-04-21 | 2018-11-30 | 华中科技大学 | A kind of g-C3N4/NiCo2S4Composite material, preparation method and applications |
CN107475745A (en) * | 2017-08-23 | 2017-12-15 | 黄河科技学院 | Phosphorus doping nitridation carbon composite modified titanic oxide optoelectronic pole, its preparation method and the application of a kind of gold modification |
CN107475745B (en) * | 2017-08-23 | 2018-12-25 | 黄河科技学院 | A kind of phosphorus doping nitridation carbon composite modified titanic oxide optoelectronic pole, preparation method and the application of gold modification |
CN108212190A (en) * | 2017-12-29 | 2018-06-29 | 长沙理工大学 | A kind of Ag bases three-dimensional sea urchin shape E-g-C3N4/ TiO2 composite materials and preparation method thereof |
CN109183192A (en) * | 2018-09-05 | 2019-01-11 | 广州小楠科技有限公司 | A kind of polyester fiber for capableing of anti-infrared perspective |
CN111514914A (en) * | 2020-04-02 | 2020-08-11 | 西华师范大学 | Ag-Ni (OH)2-(g-C3N4) Composite photocatalyst and preparation method thereof |
CN113941357A (en) * | 2021-12-02 | 2022-01-18 | 塔里木大学 | Si-TiO2/g-C3N4Ternary composite photocatalytic material and preparation method thereof |
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