CN107051546B - A kind of preparation and application of Ag-RGO-CdS ternary nano compound - Google Patents
A kind of preparation and application of Ag-RGO-CdS ternary nano compound Download PDFInfo
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- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
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- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 1
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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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Abstract
The present invention relates to the preparations and application of a kind of Ag-RGO-CdS ternary nano compound, belong to photo catalytic reduction CO2Field.The method that solvent heat is respectively adopted in the present invention be prepared for CdS nanometer rods, the mode of thermochemical reduction by graphene oxide GO be reduced to reduced graphene oxide serving RGO and with CdS nanometer rods it is compound, Ag is loaded on RGO-CdS compound in conjunction with the mode of light deposition, constitutes Ag-RGO-CdS ternary nano compound.This method is easily operated, reaction condition is more mild.This material is applied to photo catalytic reduction CO2In show excellent photocatalytic activity, selectivity of product.The addition of Ag improves the activity of catalysis reaction, and the introducing of RGO promotes the enhancing of photo-reduction selectivity.The method is intended to reduce CO in atmosphere2Concentration, the substitute for inquiring into fossil energy and Efficient Development are had broad application prospects using solar energy etc..
Description
Technical field
The invention belongs to photo catalytic reduction CO2Technical field, and in particular to Ag-RGO-CdS ternary nano compound
Preparation method and its photo catalytic reduction CO2Using.
Background technique
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 prominent.Exploitation green, novel renewable energy are reduced harmful
The discharge of gas has been 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 alleviation greenhouse effects bring environmental problem and more
Mending energy crisis caused by energy shortage has important theoretical and practical significance.
Using solar energy, by CO2And H2O is converted to hydrocarbon fuel, realizes artificial light synthetic technology, 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.However photocatalysis also
Former CO2In the process, semiconductor material because photo-generate electron-hole recombination probability it is high, it is low to lead to that there is conversion ratios in photo-reduction
And the problems such as poor selectivity.Therefore, high catalytic activity, the catalyst of selectivity or co-catalyst are developed and is 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 material synthetic technology is simple, easily operated, in photo-reduction CO2Excellent catalysis is shown in the process
Activity.The excellent performance of reduced graphene oxide serving (RGO) will be applied to provide in photo-reduction technology from now on for cheap carbon-based material
Certain reference.
Summary of the invention
In order to solve the deficiencies in the prior art, the present invention provides the preparations of ternary nano compound Ag-RGO-CdS a kind of
Method has synthesized Ag-RGO-CdS ternary nano composite material, and nano composite photo-catalyst is in photo-reduction CO2Have in active testing
Good catalytic activity.It is simple that complicated instrument, method are not needed in the preparation process, it is easy to operate, it is answered conducive to its popularization
With.
In order to achieve the above purpose, the present invention is to implement by following technical solution:
The present invention is prepared for Ag-RGO-CdS ternary nano composite material, and which are mainly applied to photo catalytic reduction CO2。
The preparation method process of the nano-complex is as follows:
(1) preparation of cadmium sulfide nano-stick (CdS nanorods): according to the method for solvent heat, CdCl2For cadmium source, thiocarbamide
(or thioacetamide, L-type cysteine, Dimethyl Asian Maple) is sulphur source, and ethylenediamine is solvent, 120~180 DEG C of solvent heat, is reacted
24~96 h obtain sample centrifugation, washing, drying.
(2) thermal reduction synthesizes RGO-CdS compound: using chemical thermal reduction, taking scattered GO solution, is added
In the CdS- ethylene glycol solution stirred evenly, through 140 DEG C of 1~4 h of reflux, cooling, washing, centrifugation, drying for standby.
(3) synthesis of Ag-RGO-CdS ternary nano compound: by photo-reduction method, RGO-CdS, which is added to, to be filled
H2In the reactor of O-TEOA mixed liquor, 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.
The mass ratio of graphene oxide GO and CdS are 0.5 ~ 5:100 in step (2).
AgNO in step (3)3Mass ratio with RGO-CdS compound is 0.1 ~ 5:100.
Xenon light shining condition Wei λ≤420 nm, 1 ~ 5h of illumination.
By the Ag-RGO-CdS ternary nano composite photo-catalyst of preparation, it to be used for photo catalytic reduction CO2Active testing experiment.
Its activity experiment test condition: H is added in catalyst2In O-TEOA system, (+420 nm of 300W xenon lamp is cut under visible light illumination
Only optical filter) carry out photo catalytic reduction CO2Activity reaches the reaction time, gas-phase product is tested and analyzed in gas-chromatography.
It effect of the invention and is advantageous in that:
(1) present invention has been successfully prepared Ag-RGO-CdS tri- by solvent-thermal method, chemical thermal reduction and Photodeposition
First nano-complex.Nano-complex is subjected to photo catalytic reduction CO2Experiment test, it is with good photo-reduction as the result is shown
CO2Activity.
(2) the ternary nano compound in the present invention, sufficiently combines the good electric conductivity of RGO, the pi-conjugated key of π-in RGO
Presence, CO can be activated2Molecule；And Ag provides active site etc. in the reaction system, the two collective effect promotes light
Restore CO2Conversion to CO substantially increases the reactivity, selectivity.
(3) synthetic method is simple and easy in the present invention, and reaction condition is mild, the excellent physicochemical property of carbon-based material, favorably
In it in photo-reduction CO2It is promoted and applied in fixed transformation technology.
Detailed description of the invention
The TEM that Fig. 1 is the resulting CdS of embodiment 1 schemes.
Fig. 2 is that the TEM of the resulting RGO-CdS compound of embodiment 1 schemes.
Fig. 3 is that the HRTEM of the resulting Ag-RGO-CdS compound of embodiment 1 schemes.
Fig. 4 is obtained each sample in photo catalytic reduction CO2Active testing figure.
Specific embodiment
To enable features described above and advantage of the invention to be clearer and more comprehensible, special embodiment below, and cooperate attached drawing, make detailed
It is carefully described as follows, but the present invention is not limited thereto.
Embodiment 1
The preparation of cadmium sulfide nano-stick (CdS nanorods): according to the method for solvent heat, 2 mmol are taken
CdCl2 .2.5H2O and 6 mmol thiocarbamides are dissolved in 20 mL ethylenediamines, are sufficiently stirred and are made it dissolve.It is then transferred into the poly- of 28 mL
It in the reaction kettle of tetrafluoroethene liner, is fitted into steel bushing and is placed in baking oven through temperature programming to 160 DEG C, react 48 h.Certainly to it
So it is cooled to room temperature, it is dry in 60 DEG C of vacuum drying ovens by obtained sample with ethanol, deionized water centrifuge washing 3 times.
Thermal reduction synthesizes RGO-CdS compound: using chemical thermal reduction, weighing 100 mg CdS nanorods and adds
Enter in the round-bottomed flask for filling 50 mL ethylene glycol (EG), dispersion is sufficiently stirred, add the GO(1 mg/mL that 3 mL have dispersed)
Solution.After agitated 20 h, 140 DEG C and 3 h of reflux are heated to, is cooled to room temperature, is carried out respectively with ethyl alcohol and deionized water
Centrifuge washing, 60 DEG C of vacuum drying, obtains jade-green RGO-CdS composite sample, is denoted as 3.0wt.% RGO-CdS
(3.0RGO-CdS).
The synthesis of Ag-RGO-CdS ternary nano compound: Ag is loaded to by RGO-CdS compound by photo-reduction mode
On, it weighs 20 mg 3.0RGO-CdS and is added to and fill 16 mL H2In the reactor of O and 4 mL TEOA mixed liquors, sufficiently stir
It mixes uniformly.Then 38 are takenμL 50 mmol/L AgNO3Solution is added thereto, under visible light (xenon lamp , λ≤420 nm) illumination
1h, the centrifuge washing under ethyl alcohol and deionized water respectively by obtained sample is subsequently placed in 40 DEG C of vacuum drying ovens dry, obtains sample
Product 1.0wt.%Ag-3.0 wt.%RGO-CdS(1.0Ag-3.0RGO-CdS).
The obtained material of the present invention is applied to photo catalytic reduction CO2Active testing, specific operation process are 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 vacuum pump, vacuum pump switch is opened, pumps the foreign gas in reaction system.Vacuum pump is closed to open
It closes, by high-purity CO2Gas is filled in reaction system, is sufficiently stirred, so that CO2It is dissolved into reaction solution.CO is turned off later2Gas
Body is filled with valve, opens vacuum pump switch, takes the gas in reactor, such operation circulation 3 times away.It finally will be filled with CO2's
Reactor sealing, which is placed under the 300W xenon lamp with 420 nm optical filters, carries out illumination.After reaching the reaction time, take a certain amount of anti-
Answer the gas in device in gas-chromatography (Shimadzu, GC-2014, TCD detector and fid detector, TDX-01 pillar, argon
Gas is carrier gas) on 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 compound, and CdS nanorods is dispersed in RGO thin layer nanometer sheet, and the two is mutual
It is in close contact.Fig. 3 is Ag-RGO-CdS sample high power transmission electron microscope picture, wherein obviously observing the lattice fringe of sample, crystal face
0.336 nm of spacing, 0.236 nm are mutually corresponded with (002) of CdS 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 are 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, the simple and mechanical mixture of RGO and CdS three.Histogram in figure respectively indicates CO2
Photo-reduction product CO and H2Production quantity；And 0.21μMol, 9.3% respectively indicates CO after CdS Nanorods Samples react 1 hour
Production quantity and product CO selectivity (CO production quantity/(CO production quantity+H2Production quantity)), other corresponding datas indicate and so on.
The foregoing is merely preferred embodiments of the invention, it is all according to the equivalent change done in scope of the present invention patent with
Modification all should belong to covering scope of the invention.
Claims (5)
- The preparation method of 1.Ag-RGO-CdS ternary nano compound, it is characterised in that:(1) preparation of CdS nanometer rods: with CdCl2For cadmium source, sulphur source is thiocarbamide, thioacetamide, L-type cysteine, diformazan Asia Any one of maple, ethylenediamine are solvent, 120~180 DEG C of solvent heat, react 24~96 h, obtain sample centrifugation, washing, dry It is dry, it is dispersed in ethylene glycol, it is spare；(2) thermal reduction synthesizes RGO-CdS compound: using chemical thermal reduction, taking scattered graphene oxidation first Object GO solution, is added in the CdS- ethylene glycol solution stirred evenly, through 140 DEG C of 1~4 h of reflux, cooling, washing, centrifugation, drying RGO-CdS compound is obtained, wherein RGO system reduced graphene oxide serving；(3) synthesis of Ag-RGO-CdS ternary nano compound: by photo-reduction method, RGO-CdS is added to fills first H2In the reactor of O-TEOA mixed liquor, 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 nano compound according to claim 1, it is characterised in that: step (2) mass ratio of graphene oxide GO and CdS are 0.5 ~ 5:100 in.
- 3. the preparation method of Ag-RGO-CdS ternary nano compound according to claim 1, it is characterised in that: step (3) AgNO in3Mass ratio with RGO-CdS compound is 0.1 ~ 5:100.
- 4. the preparation method of Ag-RGO-CdS ternary nano compound according to claim 1, it is characterised in that: xenon lamp Illumination condition Wei λ≤420 nm, 1 ~ 5h of illumination.
- 5. the Ag-RGO-CdS ternary nano compound of method preparation as described in claim 1 is being used for photo catalytic reduction CO2On Using.
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| 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 |
| CN110040706A (en) * | 2019-05-29 | 2019-07-23 | 吉林大学 | A method of preparing ultra-fine ternary cobalt manganese phosphorus nanometer rods |
| 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 |
| CN113134368A (en) * | 2021-03-22 | 2021-07-20 | 沈阳化工大学 | CdS/Cu5FeS4Preparation and application of/RGO nano composite photocatalyst |
| CN113073344B (en) * | 2021-03-23 | 2022-02-18 | 西南科技大学 | Preparation method of silver-doped cadmium sulfide nanorod electrocatalyst |
| CN114705730B (en) * | 2022-03-18 | 2024-03-29 | 吉林大学 | Ultra-fast n-propanol 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 |
| CN105498649A (en) * | 2015-12-24 | 2016-04-20 | 四川大学 | Graphene nano particle compound aerogel microspheres and preparation method thereof |
| CN106582717A (en) * | 2016-12-16 | 2017-04-26 | 昆明理工大学 | Method for preparing GO-CdS-ZnO-porous silicon composite photocatalyst |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105498649A (en) * | 2015-12-24 | 2016-04-20 | 四川大学 | Graphene nano particle compound aerogel microspheres and preparation method thereof |
| CN106582717A (en) * | 2016-12-16 | 2017-04-26 | 昆明理工大学 | Method for preparing GO-CdS-ZnO-porous silicon composite photocatalyst |
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