CN106563473A - A high-efficiency surface plasma visible-light-induced photocatalyst composite material (Ag@AgCl)-Ni/RGO having magnetic responsibility - Google Patents
A high-efficiency surface plasma visible-light-induced photocatalyst composite material (Ag@AgCl)-Ni/RGO having magnetic responsibility Download PDFInfo
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Abstract
A high-efficiency surface plasma visible-light-induced photocatalyst composite material (Ag@AgCl)-Ni/RGO having magnetic responsibility is disclosed. Firstly, a Ni/RGO composite material is prepared through a solvothermal method and by adopting graphite oxide and nickel chloride hexahydrate as precursors and adopting glycol as a solvent; then AgCl is generated on the surface of the Ni/RGO through a precipitation-deposition method and through adopting AgNO3 as a Ag<+> source and adopting NaCl as a Cl<-> source; and the AgCl surface is partially reduced into Ag through illumination to finally form the (Ag@AgCl)-Ni/RGO composite material. Under illumination by an xenon lamp having a power of 500 W, neutral red, eosine, methylene blue, methyl orange, rhodamine B, and other types of dye can be degraded in 10 min, 20 min, 35 min, 40 min and 40 min respectively through adopting the (Ag@AgCl)-Ni/RGO as a catalyst, and the degradation rates are all higher than 95%. The visible-light-induced photocatalyst material has excellent visible light catalytic degradation effects and is suitable for catalytic degradation of organic pollutants under visible light.
Description
Technical field
The present invention relates to a kind of efficient surface plasma visible light catalyst composite with magnetic responsiveness
(Ag@AgCl)-Ni/RGO, belongs to material and prepares and organic pollutant degradation processing technology field.
Background technology
In recent years, developing rapidly with industries such as weaving, printing and dyeing, petrochemical industries, it is various containing a large amount of difficult degradations, color
Degree is big, and the discharge capacity of the high organic wastewater of COD (COD) value accordingly increases, and threaten the mankind health and
The existence of organism in water.In the case, Nano semiconductor photocatalysis technology has attracted the attention of a large number of researchers.Wherein,
Surface plasma catalysis material is the metal ----quasiconductor based on the localized surface plasmons resonance effect of noble metal
Composite photocatalyst material, this material fully combines precious metal surface plasma resonance effect and composite semiconductor light is urged
The advantage of agent.The material for wherein having a class important is Ag@AgCl catalysis materials.Nano silver grain is in visible region
Surface plasma body resonant vibration absorption, can more capture photon, dramatically increase the generation of photo-generate electron-hole, and favorably
Shift to Nano silver grain surface in light induced electron, so as to realize efficiently separating for light induced electron and hole.Electronics is to surface
Transfer cause AgCl that photoreduction will not occur, it is ensured that the highlight catalytic active and stability of catalyst.Additionally,
Because Graphene can play the connection of carrier and dispersed particle effect, and photo-generate electron-hole pair can be effectively promoted
Separate, increase adsorption of the Organic substance on surface, thus be also used for the carrier of Ag@AgCl nanoparticles, i.e.,
Ag@AgCl/RGO composites.
It is easy to reclaim the magnetic response of circulation to give photocatalyst, it is one that magnetic nano-particle is added in its structure
Plant usual way, Zhong etc. and Fe is obtained by solvent-thermal method3O4/ RGO composites, and as catalyst activity master
The carrier of body Ag@AgCl nanoparticles, obtains (Ag@AgCl)-Fe3O4/ RGO composites [Zhong S, Jiang W,
Han M,et al.Graphene supported silver@silver chloride&ferroferric oxide hybrid,a
magnetically separable photocatalyst with high performance under visible light irradiation[J].
Applied Surface Science,2015,347:242-249.].However, Fe3O4Used as a class semi-metallic, it is led
Electrically it is far below metallic conductor.In photocatalytic process, low electric conductivity can limit the migration of electric charge, so as to have influence on catalysis
Performance.
The content of the invention
For the deficiencies in the prior art, the invention provides a kind of efficient surface plasma visible ray with magnetic responsiveness
Catalyst composite (Ag@AgCl)-Ni/RGO and its preparation method and application.Ni is both metallic conductor, and with excellent
Good magnetic responsiveness, Ni/RGO can be used as the excellent carrier of photocatalyst of a class.With reference to Ag@AgCl and Ni/RGO
A kind of new efficient surface plasma visible light catalyst composite with magnetic responsiveness is obtained
(Ag@AgCl)-Ni/RGO。
The technical scheme is that：A kind of efficient surface plasma visible light catalyst composite wood with magnetic responsiveness
Material (Ag@AgCl)-Ni/RGO, is prepared by following steps：First with graphite oxide (GO) and Nickel dichloride hexahydrate
(NiCl2·6H2O it is) presoma, Ni/RGO composites is obtained by solvent-thermal method by solvent of ethylene glycol, wherein
RGO is reduced form graphite oxide, then with AgNO3For Ag+Source, with NaCl as Cl-Source, by precipitation-sedimentation
In Ni/RGO Surface Creation AgCl, illumination afterwards makes AgCl surface portion be reduced to Ag, ultimately forms
(Ag@AgCl)-Ni/RGO composites.Comprise the following steps that：
1. by graphite oxide (GO) and Nickel dichloride hexahydrate (NiCl2·6H2O) by ultrasonic disperse at ethylene glycol (EG)
Graphite oxide can be peeled off in ethylene glycol middle formation mixed dispersion liquid, ultrasonic procedure the lamellar structure for graphite oxide,
Then the hydrazine hydrate solution of NaOH is added dropwise over, solvent thermal reaction is carried out, that is, obtains Ni/RGO composites；
2. in dark room conditions, Ni/RGO is dispersed in into AgNO3In solution, adsorbed, then Deca and AgNO3
The NaCl solution of equimolar amountss, so as to generate AgCl in Ni/RGO surfaces precipitation-deposition；
3. xenon lamp irradiates above-mentioned mixed liquor under stirring condition, and AgCl surface portion is reduced to Ag, ultimately forms
(Ag@AgCl)-Ni/RGO composites.
Step 1. in, GO and NiCl2·6H2O mass ratioes are 50:118～236, ultrasonic time is 60min～120min,
Ethylene glycol is 6～7 with the volume ratio of the hydrazine hydrate solution of NaOH:1, NaOH hydrazine hydrate solution concentration is
0.05～0.10g/mL.
Step 1. in, the solvent thermal time be 45min～60min.
Step 2. in, adsorption time be 30min～60min, AgNO3With NiCl2·6H2The mol ratio of O is 1～2:1.
Step 3. in, light application time be 5min～10min.
Compared with prior art, remarkable advantage of the invention is as follows：
1. carrier Ni/RGO has superior electrical conductivity, is conducive to the transmission of carrier in catalytic process, improves catalytic performance；
2. visible light catalyst (Ag@AgCl)-Ni/RGO microstructures are acanthosphere shape, possess a large amount of corners and tip former
Son, there is provided more avtive spots；
3. visible light catalyst (Ag@AgCl)-Ni/RGO catalytic performances are good, high catalytic efficiency；
4. visible light catalyst (Ag@AgCl)-Ni/RGO magnetic responsivenesses are good, and stability is high, can be recycled.
Description of the drawings
Fig. 1 is the transmission electron microscope of visible light catalyst composite (Ag@the AgCl)-Ni/RGO of gained in embodiment 1
Figure.
Fig. 2 is visible light catalyst composite (Ag@the AgCl)-Ni/RGO and its intermediate product of gained in embodiment 1
XRD diffraction spectrograms.
Fig. 3 is the VSM figures of visible light catalyst composite (Ag@the AgCl)-Ni/RGO of gained in embodiment 1.
Fig. 4 is visible light catalyst composite (Ag@the AgCl)-Ni/RGO of gained in embodiment 1 to different dyes
Degradation curve figure, is followed successively by from left to right dimethyl diaminophenazine chloride, eosin, methylene blue, methyl orange, rhodamine B.
Fig. 5 be (Ag@AgCl)/RGO obtained in (Ag@AgCl)-Ni/RGO, comparative example 1 obtained in embodiment 1 and
(Ag@AgCl)-Fe obtained in comparative example 23O4The degraded comparison diagrams of/RGO to methylene blue.
Specific embodiment
Embodiment 1：The preparation of visible light catalyst composite (Ag@AgCl)-Ni/RGO
0.05g graphite oxides (GO), 0.118g NiCl are weighed successively2·6H2O, ultrasonic disperse in 70mL ethylene glycol,
Ultrasonic time is 60min.Then under the auxiliary of magnetic agitation, it is added dropwise over 10mL and is dissolved with 0.5g NaOH's
Hydrazine hydrate (N2H4·H2O, 80wt%) solution.Continue to stir after 15min, the mixed liquor is proceeded to into 100mL reactions
Kettle, at 200 DEG C 45min is reacted.Solvent thermal reaction terminates, and after this intermediate product is cooled down at room temperature, uses repeatedly
Ethanol and water are cleaned, and obtain Ni/RGO composites.
Under dark room conditions, intermediate product Ni/RGO is dispersed in into 40mL comprising 0.17g AgNO3Aqueous solution in, machine
After tool stirring 30min, aqueous solutions of the 10mL comprising 0.059g NaCl is slowly added dropwise.Continue at and stirred under dark room conditions
After mixing 12h, 5min is irradiated with 500W xenon lamps, obtain final product end-product (Ag@AgCl)-Ni/RGO composites.
As seen from Figure 1, particle diameter is about the nanoparticle of the acanthosphere shape of 70nm and is evenly dispersed on Graphene.Figure
2 is the XRD figure of products obtained therefrom, it may be determined that the presence of Ag, AgCl, Ni and RGO in product.From the figure 3, it may be seen that
The saturation magnetization and coercive field intensity of (Ag AgCl)-Ni/RGO is respectively 9.5emug-1And 190.7Oe.Fig. 3
In illustration, homodisperse catalyst can rapidly be separated under Magnet effect in solution.
Embodiment 2：The preparation of visible light catalyst composite (Ag@AgCl)-Ni/RGO
0.05g graphite oxides (GO), 0.118g NiCl are weighed successively2·6H2O, ultrasonic disperse in 60mL ethylene glycol,
Ultrasonic time is 90min.Then under the auxiliary of magnetic agitation, it is added dropwise over 10mL and is dissolved with 0.5g NaOH's
Hydrazine hydrate ((N2H4·H2O, 80wt%)) solution.Continue to stir after 15min, the mixed liquor is proceeded to into 100mL anti-
Kettle is answered, at 200 DEG C 60min is reacted.Solvent thermal reaction terminates, after this intermediate product is cooled down at room temperature, repeatedly
Cleaned with ethanol and water, obtain Ni/RGO composites.
Under dark room conditions, intermediate product Ni/RGO is dispersed in into 40mL comprising 0.17g AgNO3Aqueous solution in, machine
After tool stirring 30min, aqueous solutions of the 10mL comprising 0.059g NaCl is slowly added dropwise.Continue at and stirred under dark room conditions
After mixing 12h, 5min is irradiated with 500W xenon lamps, obtain final product end-product (Ag@AgCl)-Ni/RGO composites.
Embodiment 3：The preparation of visible light catalyst composite (Ag@AgCl)-Ni/RGO
0.05g graphite oxides (GO), 0.236g NiCl are weighed successively2·6H2O, ultrasonic disperse in 70mL ethylene glycol,
Ultrasonic time is 120min.Then under the auxiliary of magnetic agitation, it is added dropwise over 10mL and is dissolved with 1.0g NaOH's
Hydrazine hydrate (N2H4·H2O, 80wt%) solution.Continue to stir after 15min, the mixed liquor is proceeded to into 100mL reactions
Kettle, at 200 DEG C 45min is reacted.Solvent thermal reaction terminates, and after this intermediate product is cooled down at room temperature, uses repeatedly
Ethanol and water are cleaned, and obtain Ni/RGO composites.
Under dark room conditions, intermediate product Ni/RGO is dispersed in into 40mL comprising 0.17g AgNO3Aqueous solution in, machine
After tool stirring 60min, aqueous solutions of the 10mL comprising 0.059g NaCl is slowly added dropwise.Continue at and stirred under dark room conditions
After mixing 12h, 10min is irradiated with 500W xenon lamps, obtain final product end-product (Ag@AgCl)-Ni/RGO composites.
Embodiment 4：Visible light catalyst composite (the Ag@AgCl) degradeds of-Ni/RGO to different dyes
The photocatalysis performance of photocatalyst (Ag@the AgCl)-Ni/RGO of the gained of embodiment 1 in the case where visible ray shines by urging
Change degraded dimethyl diaminophenazine chloride (NR), eosin (Eosin), methylene blue (MB), methyl orange (MO), rhodamine B (RB)
Five kinds of dyestuffs are determining.50mg (Ag@AgCl)-Ni/RGO is weighed in photocatalysis pipe, 50mL dye solutions are added
(10mg/L), after lucifuge stirring 60min, react under the irradiation of 500W xenon lamps.In degradation process, when one section
Between, 3mL sample liquid is taken, after removing catalyst, using ultraviolet-uisible spectrophotometer dye strength in sample liquid is determined.
Visible light catalyst composite (Ag@AgCl)-Ni/RGO to the degradation curve figure of different dyes as shown in figure 4,
Can respectively in 10min, 20min, 35min, 40min and 40min degrade dimethyl diaminophenazine chloride, eosin, methylene blue,
The dyestuff such as methyl orange and rhodamine B, and degradation rate is more than 95%.As can be seen here, the catalyst material has substantially excellent
Different visible light photocatalytic degradation effect.
Comparative example 1：The preparation of visible light catalyst composite (Ag@AgCl)/RGO
0.05g graphite oxides (GO) are weighed, in 70mL ethylene glycol, ultrasonic time is 90min to ultrasonic disperse.Then
Under the auxiliary of magnetic agitation, the hydrazine hydrate ((N that 10mL is dissolved with 0.5g NaOH is added dropwise over2H4·H2O,80
Wt%)) solution.Continue to stir after 15min, the mixed liquor is proceeded to into 100mL reactors, at 200 DEG C 45 are reacted
min.Solvent thermal reaction terminates, and after this intermediate product is cooled down at room temperature, is cleaned with ethanol and water repeatedly, obtains RGO
Composite.
Under dark room conditions, intermediate product RGO is dispersed in into 40mL comprising 0.17g AgNO3Aqueous solution in, machinery
After stirring 30min, aqueous solutions of the 10mL comprising 0.059g NaCl is slowly added dropwise.Continue at and stirred under dark room conditions
After 12h, 5min is irradiated with 500W xenon lamps, obtain final product end-product (Ag@AgCl)/RGO composites.
Comparative example 2：Visible light catalyst composite (Ag@AgCl)-Fe3O4The preparation of/RGO
Weigh 0.05g graphite oxides (GO) successively, 1.0g Polyethylene Glycol (PEG4000), ultrasonic disperse is in 80mL
Ethylene glycol, ultrasonic time is 120min.Then 0.27g FeCl are added3·6H2O and 1g NaAc, continue ultrasound 30
min.The mixed liquor is proceeded to into 100mL reactors, at 200 DEG C 10h is reacted.Solvent thermal reaction terminates, by this
Between after product cools down at room temperature, cleaned with ethanol and water repeatedly, obtain Fe3O4/ RGO composites.
Under dark room conditions, by intermediate product Fe3O4/ RGO is dispersed in 40mL comprising 0.17g AgNO3Aqueous solution in,
After mechanical agitation 30min, aqueous solutions of the 10mL comprising 0.059g NaCl is slowly added dropwise.Under continuing at dark room conditions
After stirring 12h, 5min is irradiated with 500W xenon lamps, obtain final product end-product (Ag@AgCl)-Fe3O4/ RGO composites.
Embodiment 5：
Weigh (Ag@AgCl)/RGO obtained in (Ag@AgCl)-Ni/RGO, comparative example 1 obtained in 50mg embodiments 1,
(Ag@AgCl)-Fe obtained in comparative example 23O4/ RGO adds 50mL methylene blue solutions (10 in photocatalysis pipe
Mg/L), after lucifuge stirring 60min, react under the irradiation of 500W xenon lamps.
Embodiment 1 is contrasted with the catalytic performance of the product of comparative example 1,2 by degradation of methylene blue solution, such as Fig. 5 institutes
Show.The introducing of magnetic particle can reduce product catalysis activity, (Ag@AgCl)-Ni/RGO compare (Ag@AgCl)-
Fe3O4/ RGO, its photocatalytic activity is much closer to non-magnetic (Ag@AgCl)/RGO.This is because
In (Ag@AgCl)/RGO, Ag@AgCl and RGO directly contacts, and RGO light transmissions are good, this is conducive to Ag@AgCl
Effective absorption of the particle to light, so as to have maximum photocatalytic activity.On the other hand, the electric conductivity of Ni/RGO is much larger than
Fe3O4/ RGO, carrier can be transmitted preferably wherein, so that (Ag@AgCl)-Ni/RGO photocatalytic activities
It is much better than (Ag@AgCl)-Fe3O4/RGO。
Claims (6)
1. a kind of efficient surface plasma visible light catalyst composite with magnetic responsiveness
(Ag@AgCl)-Ni/RGO, it is characterised in that prepared by following steps：First with graphite oxide and six chloride hydrates
Nickel is presoma, Ni/RGO composites is obtained by solvent-thermal method by solvent of ethylene glycol, then with AgNO3For
Ag+Source, with NaCl as Cl-Source, by precipitation-sedimentation in Ni/RGO Surface Creation AgCl, illumination afterwards makes AgCl
Surface portion is reduced to Ag, ultimately forms (Ag@AgCl)-Ni/RGO composites.
2. prepare the efficient surface plasma visible light catalyst with magnetic responsiveness as claimed in claim 1 to be combined
The method of material (Ag@AgCl)-Ni/RGO, it is characterised in that comprise the following steps that：
Step 1, forms mixed dispersion liquid, so by ultrasonic disperse by graphite oxide and Nickel dichloride hexahydrate in ethylene glycol
The hydrazine hydrate solution of NaOH is added dropwise over afterwards, solvent thermal reaction is carried out, that is, obtain Ni/RGO composites；
Step 2, in dark room conditions, by Ni/RGO AgNO is dispersed in3In solution, adsorbed, then Deca with
AgNO3The NaCl solution of equimolar amountss, on Ni/RGO surfaces, precipitation-deposition generates AgCl；
Step 3, the mixed liquor of the gained of xenon lamp irradiating step 2 under stirring condition, AgCl surface portion is reduced to Ag,
Ultimately form (Ag@AgCl)-Ni/RGO composites.
3. preparation method according to claim 2, it is characterised in that in step 1, described graphite oxide and six
The mass ratio of hydrated nickel chloride is 50:118～236, ultrasonic time is 60min～120min, described ethylene glycol with
The volume ratio of the hydrazine hydrate solution of NaOH is 6～7:1, NaOH hydrazine hydrate solution concentration is 0.05～0.10g/mL, molten
The agent thermal response time is 45min～60min.
4. preparation method according to claim 2, it is characterised in that in step 2, adsorption time be 30min～
60min, described AgNO3With NiCl2·6H2The mol ratio of O is 1～2:1.
5. preparation method according to claim 2, it is characterised in that in step 3, light application time is 5min～10
min。
6. the efficient surface plasma visible light catalyst composite wood with magnetic responsiveness according to claim 1
The application of material (Ag@AgCl)-Ni/RGO, it is characterised in that suitable for catalytic degradation organic pollution under visible ray.
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| CN106975499A (en) * | 2017-05-05 | 2017-07-25 | 董可轶 | A kind of Ag@AgCl/rGO sandwich nano composite materials and preparation method and application |
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| CN112237925A (en) * | 2019-07-17 | 2021-01-19 | 南京凯旋化学科技有限公司 | Catalytic material for degrading organic matters in wastewater and preparation method thereof |
| CN111769297B (en) * | 2020-07-17 | 2022-08-16 | 郑州佛光发电设备股份有限公司 | Cathode catalyst of aluminum-air battery and preparation method thereof |
| CN114950498A (en) * | 2022-05-16 | 2022-08-30 | 江苏农林职业技术学院 | Recyclable efficient photocatalytic material and preparation method and application thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106975499A (en) * | 2017-05-05 | 2017-07-25 | 董可轶 | A kind of Ag@AgCl/rGO sandwich nano composite materials and preparation method and application |
| CN108940324A (en) * | 2018-07-20 | 2018-12-07 | 宝鸡文理学院 | A kind of multi-walled carbon nanotube-Ag@AgCl composite nano materials and preparation method thereof with photocatalytic |
| CN112237925A (en) * | 2019-07-17 | 2021-01-19 | 南京凯旋化学科技有限公司 | Catalytic material for degrading organic matters in wastewater and preparation method thereof |
| CN111769297B (en) * | 2020-07-17 | 2022-08-16 | 郑州佛光发电设备股份有限公司 | Cathode catalyst of aluminum-air battery and preparation method thereof |
| CN114950498A (en) * | 2022-05-16 | 2022-08-30 | 江苏农林职业技术学院 | Recyclable efficient photocatalytic material and preparation method and application thereof |
| CN114950498B (en) * | 2022-05-16 | 2023-12-22 | 江苏农林职业技术学院 | Recyclable efficient photocatalytic material and preparation method and application thereof |
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