CN107051546A - A kind of preparation and application of Ag RGO CdS ternary nano compounds - Google Patents
A kind of preparation and application of Ag RGO CdS ternary nano compounds Download PDFInfo
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- 239000005864 Sulphur Substances 0.000 claims description 2
- 229910052793 cadmium Inorganic materials 0.000 claims description 2
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 2
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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
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
-
- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/48—Silver or gold
- B01J23/50—Silver
-
- 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
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
- Y02P20/133—Renewable energy sources, e.g. sunlight
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The present invention relates to a kind of preparation and application of Ag RGO CdS ternary nano compounds, belong to photo catalytic reduction CO2Field.The method that solvent heat is respectively adopted in the present invention is prepared for CdS nanometer rods, the mode of thermochemical reduction graphene oxide GO is reduced into reduced graphene oxide serving RGO and is combined with CdS nanometer rods, Ag is loaded on RGO CdS compounds with reference to the mode of light deposition, Ag RGO CdS ternary nano compounds are constituted.This method is easily operated, reaction condition is more gentle.This materials application is in photo catalytic reduction CO2In show excellent photocatalytic activity, selectivity of product.Ag addition improves the activity of catalytic reaction, and RGO introducing promotes the enhancing of photo-reduction selectivity.The method is intended to CO in reduction air2Concentration, the substitute and Efficient Development of fossil energy are inquired into using being had broad application prospects in terms of solar energy.
Description
Technical field
The invention belongs to photo catalytic reduction CO2Technical field, and in particular to Ag-RGO-CdS ternary nano compounds
Preparation method and its photo catalytic reduction CO2Using.
Technical background
With the fast development of economic society level, the lasting consumption of non-renewable fossil fuel, the mankind are to energy demand
Increasingly increase so that environmental pollution and problem of energy crisis are increasingly highlighted.Exploitation green, novel renewable energy, are reduced harmful
The discharge of gas is very urgent.Under the driving of solar energy, using Photocatalitic Technique of Semiconductor, by CO2Photocatalytic conversion
For useful CO, CH4, HCOOH, CH3The hydrocarbon fuels such as OH and HCHO, for alleviating the environmental problem brought of greenhouse effects and more
Energy crisis caused by mending energy shortage has important theoretical and practical significance.
Using solar energy, by CO2And H2O is converted to hydrocarbon fuel, realizes artificial light synthetic technology, and this will be expected to acquirement can
Lasting energy conversion, and can be considered the broad road for changing and relying on conventional fossil fuel.But in photocatalysis also
Former CO2During, semi-conducting material is high because of photo-generate electron-hole recombination probability, causes to there is conversion ratio in photo-reduction low
And the problems such as poor selectivity.Therefore, exploitation high catalytic activity, the catalyst of selectivity or co-catalyst are applied to photo-reduction CO2
System seems most important.
Design has synthesized ternary nano composite photo-catalyst in the present invention, investigates it in photo catalytic reduction CO2In system
Performance interactively.Composite synthetic technology is simple, easily operated, in photo-reduction CO2During show excellent catalysis
Activity.Reduced graphene oxide serving（RGO）Excellent performance, is that cheap carbon-based material will be applied to provide in photo-reduction technology from now on
Certain reference.
The content of the invention
In order to solve the deficiencies in the prior art, the invention provides a kind of ternary nano compound Ag-RGO-CdS preparation
Method, has synthesized Ag-RGO-CdS ternary nano composite materials, nano composite photo-catalyst is in photo-reduction CO2Have in active testing
Good catalytic activity.Do not need complicated instrument, method simple in the preparation process, easily operation, being promoted beneficial to it should
With.
In order to realize above-mentioned purpose, the present invention is to be implemented by following technical solution：
The present invention is prepared for Ag-RGO-CdS ternary nano composite materials, and it is mainly used in photo catalytic reduction CO2。
The preparation method process of the nano-complex is as follows：
（1）Cadmium sulfide nano-stick（CdS nanorods）Preparation：According to the method for solvent heat, CdCl2For cadmium source, thiocarbamide（Or
Thioacetamide, L-type cysteine, DMSO）For sulphur source, ethylenediamine is solvent, 120~180 DEG C of solvent heat, reaction 24~
96 h, obtain sample centrifugation, washing, drying.
（2）Thermal reduction synthesizes RGO-CdS compounds：Using chemical thermal reduction, scattered GO solution is taken, is added
In the CdS- ethylene glycol solutions stirred, through 140 DEG C of 1~4 h of backflow, cooling, washing, centrifugation, drying for standby.
（3）The synthesis of Ag-RGO-CdS ternary nano compounds：By photo-reduction method, RGO-CdS, which is added to, to be filled
H2In the reactor of O-TEOA mixed liquors, stir.Then AgNO is taken3Solution is added thereto, Xenon light shining, will be obtained
Sample centrifuge washing, be subsequently placed in dry dry in baking oven.
By the Ag-RGO-CdS ternary nano composite photo-catalysts of preparation, for photo catalytic reduction CO2Active testing is tested.
Its activity experiment test condition：Catalyst adds H2In O-TEOA systems, under visible light illumination（The nm of 300W xenon lamps+420 is cut
Only optical filter）Carry out photo catalytic reduction CO2Activity, reaches the reaction time, gas-phase product is tested and analyzed in gas-chromatography.
The present invention effect and be advantageous in that：
（1）The present invention has been successfully prepared Ag-RGO-CdS ternarys and received by solvent-thermal method, chemical thermal reduction and Photodeposition
Rice compound.Nano-complex is subjected to photo catalytic reduction CO2Experiment test, as a result shows that it has good photo-reduction CO2's
Activity.
（2）Ternary nano compound in the present invention, fully combines π-pi-conjugated key in the good electric conductivity of RGO, RGO
Presence, CO can be activated2Molecule；And Ag provides avtive spot etc. in reaction system, both promote light at collective effect
Reduce CO2To CO conversion, the reactivity, selectivity are substantially increased.
（3）Synthetic method is simple and easy to apply in the present invention, and reaction condition is gentle, the excellent physicochemical property of carbon-based material, favorably
In it in photo-reduction CO2Popularization and application in fixed transformation technology.
Brief description of the drawings
The TEM figures that Fig. 1 is the CdS of the gained of embodiment 1.
Fig. 2 is the TEM figures of the RGO-CdS compounds of the gained of embodiment 1.
Fig. 3 is the HRTEM figures of the Ag-RGO-CdS compounds of the gained of embodiment 1.
Fig. 4 is resulting each sample in photo catalytic reduction CO2Active testing figure.
Embodiment
To enable the features described above and advantage of the present invention to become apparent, special embodiment below, and coordinate accompanying drawing, make detailed
Carefully it is described as follows, but the present invention is not limited thereto.
Embodiment 1
Cadmium sulfide nano-stick（CdS nanorods）Preparation：According to the method for solvent heat, 2 mmol CdCl are taken2 .2.5H2O and 6
Mmol thiocarbamides are dissolved in 20 mL ethylenediamines, are sufficiently stirred for dissolving it.It is then transferred into 28 mL polytetrafluoroethyllining lining
In reactor, it is fitted into steel bushing and is placed in baking oven through temperature programming to 160 DEG C, reacts 48 h., will after it is down to room temperature naturally
Resulting sample with ethanol, deionized water centrifuge washing 3 times, are dried in 60 DEG C of vacuum drying ovens.
Thermal reduction synthesizes RGO-CdS compounds：Using chemical thermal reduction, weigh 100 mg CdS nanorods and add
Enter to fill 50 mL ethylene glycol（EG）Round-bottomed flask in, be sufficiently stirred for disperseing, add the GO that 3 mL have disperseed（1 mg/mL）
Solution.After agitated 20 h, 140 DEG C and 3 h of backflow are heated to, room temperature is cooled to, is carried out respectively with ethanol and deionized water
Centrifuge washing, 60 DEG C of vacuum drying, obtains jade-green RGO-CdS composite samples, is designated as 3.0wt.% RGO-CdS
（3.0RGO-CdS）.
The synthesis of Ag-RGO-CdS ternary nano compounds：Ag is loaded to by RGO-CdS compounds by photo-reduction mode
On, weigh 20 mg 3.0RGO-CdS and be added to and fill 16 mL H2In the reactor of O and 4 mL TEOA mixed liquors, fully stir
Mix uniform.Then 38 are takenμL 50 mmol/L AgNO3Solution is added thereto, under visible light（The nm of xenon lamp , λ≤420）Illumination
1h, by the obtained sample centrifuge washing under ethanol and deionized water respectively, is subsequently placed in 40 DEG C of vacuum drying ovens and dries, obtain sample
Product 1.0wt.%Ag-3.0 wt.%RGO-CdS（1.0Ag-3.0RGO-CdS）.
Materials application obtained by the present invention is in photo catalytic reduction CO2Active testing, specific operation process is as follows：
Weigh catalyst sample made from 5 mg embodiments 1,4 mL H2O, 2 mL TEOA are added in 80 mL reactors, sealing.
Reactor is accessed into vavuum pump, vacuum pump switch is opened, pumps the foreign gas in reaction system.Vacuum pump switch is closed, will
High-purity CO2Gas is filled with reaction system, is sufficiently stirred for so that CO2It is dissolved into reaction solution.CO is turned off afterwards2Gas is filled with
Valve, opens vacuum pump switch, takes the gas in reactor away, such operation circulation 3 times.It finally will be filled with CO2Reactor
Sealing, which is placed under the 300W xenon lamps with 420 nm optical filters, carries out illumination.Reach after the reaction time, take in a certain amount of reactor
Gas in gas-chromatography（Shimadzu, GC-2014, TCD detector and fid detector, TDX-01 pillars, argon gas is load
Gas）Upper carry out reaction product（CO and H2）Analysis.
Fig. 1 is the transmission electron microscope picture of CdS nanometer rods, is clear that in figure that CdS is deposited in the form of nanometer rods
.Fig. 2 is the transmission electron microscope picture of RGO-CdS compounds, and CdS nanorods are dispersed in RGO thin layer nanometer sheets, and both are mutual
It is in close contact.Fig. 3 is Ag-RGO-CdS sample high power transmission electron microscope pictures, wherein substantially observing the lattice fringe of sample, crystal face
The nm of spacing 0.336,0.236 nm are mutually corresponded with CdS (002) and Ag (111) crystal face respectively, and Ag, RGO and CdS tri-
Person is closely contacted with each other.Fig. 4 is the photo-reduction CO of sample2Catalytic activity figure, sample is CdS nanorods, 1.0 respectivelywt.%
Ag-CdS (1.0Ag-CdS)、3.0 wt.%RGO-CdS(3.0RGO-CdS)、1.0 wt.%Ag-3.0 wt.%RGO-CdS
(1.0Ag-3.0RGO-CdS) and Ag, RGO and CdS three simple and mechanical mixture.Block diagram in figure represents CO respectively2
Photo-reduction product CO and H2Growing amount；And 0.21μMol, 9.3% respectively represent CdS Nanorods Samples react 1 hour after CO
Growing amount and product CO selectivity (CO growing amounts/(CO growing amounts+H2Growing amount)), other corresponding datas are represented by that analogy.
The foregoing is only the present invention preferred embodiments, it is all according to the equivalent change done in scope of the present invention patent with
Modification should all belong to the covering scope of the present invention.
Claims (5)
1. the preparation method of Ag-RGO-CdS ternary nano compounds, it is characterised in that：
（1）The preparation of CdS nanometer rods：With CdCl2For cadmium source, sulphur source is thiocarbamide, thioacetamide, L-type cysteine, diformazan Asia
Any of maple, ethylenediamine is solvent, and 120~180 DEG C of solvent heat reacts 24~96 h, obtains sample centrifugation, washing, dries
It is dry, it is dispersed in ethylene glycol, it is standby；
（2）Thermal reduction synthesizes RGO-CdS compounds：Using chemical thermal reduction, scattered graphene is taken to aoxidize first
Thing GO solution, is added in the CdS- ethylene glycol solutions stirred, through 140 DEG C of 1~4 h of backflow, is cooled down, washs, centrifuges, is dried
Obtain RGO-CdS compounds, wherein RGO systems reduced graphene oxide serving；
（3）The synthesis of Ag-RGO-CdS ternary nano compounds：By photo-reduction method, RGO-CdS is added to filled first
H2In the reactor of O-TEOA mixed liquors, stir；Then AgNO is taken3Solution is added thereto, Xenon light shining, will be obtained
Sample centrifuge washing, be placed in baking oven dry.
2. the preparation method of Ag-RGO-CdS ternary nanos compound according to claim 1, it is characterised in that：Step
（2）Middle graphene oxide GO and CdS mass ratio is 0.5 ~ 5:100.
3. the preparation method of Ag-RGO-CdS ternary nanos compound according to claim 1, it is characterised in that：Step
（3）Middle AgNO3Mass ratio with RGO-CdS compounds is 0.1 ~ 5:100.
4. the preparation method of Ag-RGO-CdS ternary nanos compound according to claim 1, it is characterised in that：Xenon lamp
Illumination condition Wei λ≤420 nm, 1 ~ 5h of illumination.
5. Ag-RGO-CdS ternary nanos compound prepared by method as claimed in claim 1 is for photocatalysis CO2On should
With.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109954508A (en) * | 2019-04-17 | 2019-07-02 | 南昌航空大学 | A kind of composite photocatalyst material and its preparation method and application |
| CN110040706A (en) * | 2019-05-29 | 2019-07-23 | 吉林大学 | A method of preparing ultra-fine ternary cobalt manganese phosphorus nanometer rods |
| CN110064410A (en) * | 2019-05-10 | 2019-07-30 | 深圳大学 | A method of it is extremely easy to prepare the monatomic catalyst of noble metal |
| CN111298789A (en) * | 2020-02-25 | 2020-06-19 | 福建生物工程职业技术学院 | Au/RGO composite aerogel and preparation method and application thereof |
| CN111939933A (en) * | 2020-07-16 | 2020-11-17 | 沈阳化工大学 | Preparation method of ternary stepped heterojunction semiconductor photocatalyst |
| CN113073344A (en) * | 2021-03-23 | 2021-07-06 | 西南科技大学 | Preparation method of silver-doped cadmium sulfide nanorod electrocatalyst |
| CN113134368A (en) * | 2021-03-22 | 2021-07-20 | 沈阳化工大学 | CdS/Cu5FeS4Preparation and application of/RGO nano composite photocatalyst |
| CN114705730A (en) * | 2022-03-18 | 2022-07-05 | 吉林大学 | Ultrafast normal propyl alcohol sensor based on CdS/rGO nano sensitive material and preparation method thereof |
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| WO2014120722A1 (en) * | 2013-01-31 | 2014-08-07 | Sunpower Technologies Llc | Photocatalyst for the reduction of carbon dioxide |
| CN105363477A (en) * | 2015-10-23 | 2016-03-02 | 南昌航空大学 | Method for preparing silver/cadmium sulfide/titanium dioxide composite photocatalytic material |
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