CN105688957A - CNTs-Ag3PO4 catalyst with visible light catalytic activity and preparation method of catalyst - Google Patents
CNTs-Ag3PO4 catalyst with visible light catalytic activity and preparation method of catalyst Download PDFInfo
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- CN105688957A CN105688957A CN201610204641.8A CN201610204641A CN105688957A CN 105688957 A CN105688957 A CN 105688957A CN 201610204641 A CN201610204641 A CN 201610204641A CN 105688957 A CN105688957 A CN 105688957A
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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
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/16—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr
- B01J27/18—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr with metals other than Al or Zr
- B01J27/1802—Salts or mixtures of anhydrides with compounds of other metals than V, Nb, Ta, Cr, Mo, W, Mn, Tc, Re, e.g. phosphates, thiophosphates
- B01J27/1817—Salts or mixtures of anhydrides with compounds of other metals than V, Nb, Ta, Cr, Mo, W, Mn, Tc, Re, e.g. phosphates, thiophosphates with copper, silver or gold
Abstract
The invention discloses a carbon nano tube-Ag3PO4 composite catalyst which is prepared by uniformly mixing aqueous dispersion of carbon nano tubes (CNTs) with Ag3PO4 aqueous suspension and performing hydrothermal treatment under the temperature of 120 to 180 DEG C for 4 to 24 hours. The carbon nano tube-Ag3PO4 composite catalyst has the beneficial effect that a silver phosphate-based photocatalyst with high stability and high catalysis activity can be synthesized by a low-cost and simple preparation method. The invention discloses a preparation method of the carbon nano tube-Ag3PO4 composite catalyst.
Description
Technical field
The present invention relates to the synthetic catalyst with visible light catalysis activity, particularly to material with carbon element-Ag3PO4Composite catalyst。
Background technology
Photocatalysis technology is to utilize illumination and catalyst combined effect, photochemical reaction occurs, has certain advantage for being difficult to biodegradable organic matter removal。1972, Fujishima and Honda was found that TiO2Single Crystalline Electrodes can in this phenomenon of decomposition water under light action, and this is to utilizing solar energy, and the shortage solving fossil energy has great importance。Since then, photocatalysis technology enters brand-new epoch。Afterwards, photocatalytic applications is appeared in the newspapers repeatly in the research of environmental pollution improvement's aspect, is developed rapidly removing the environmental photocatlytsis technology that environmental contaminants are main purpose。In recent years, the emergence of nanotechnology and the development of characterization method, also promote the development of photocatalysis technology further。
Ag3PO4Photocatalyst has attracted the interest of more and more researcher because of the visible light catalytic performance of its brilliance, becomes one of focus of current visible light catalyst research direction。Although improving Ag3PO4Photocatalyst visible light catalysis activity and chemical stability aspect researcher have done a lot of work, but it is relatively costly to be because Ag series material, from the angle of practical application, utilize Ag or Ag series material to carry out compound Ag3PO4It it is not optimal method；Compound Ag is carried out with oxide3PO4, can put forward high catalytic activity or stability to a certain extent, but Ag mostly3PO4/ oxide catalyst while improving photocatalytic activity, can not also strengthen its chemical stability；Material with carbon element-Ag is prepared for carrier with material with carbon element3PO4Photocatalyst, can carry high catalytic activity, can strengthen catalyst chemical stability simultaneously, but at present it have been reported that material with carbon element Ag3PO4Preparation method needs to add surfactant mostly, and preparation process is comparatively laborious。Therefore with the silver phosphate based photocatalyst of the friendly high stability of relatively low cost, simple preparation method synthetic environment and high catalytic activity, it is still following be badly in need of solving and the work of great meaning。
Summary of the invention
It is an object of the invention to provide a kind of high catalytic activity and the good material with carbon element-Ag of chemical stability3PO4Photocatalyst and its relatively low cost, simple preparation method。
Technical scheme is as follows:
A kind of CNT-Ag3PO4Composite catalyst, it is by the aqueous dispersions of CNT (CNTs) and Ag3PO4Aqueous suspension mix homogeneously, at 120 DEG C-180 DEG C CNT-Ag obtained for hydro-thermal 4-24 hour3PO4Composite catalyst。
Above-mentioned composite catalyst, described CNT and Ag3PO4Mass ratio is 1:10 1:30。
A kind of above-mentioned CNTs-Ag3PO4The preparation method of catalyst, it is characterised in that comprise the following steps:
Step 1, the CNTs weighing certain mass are put in the beaker filling 30mL distilled water, after ultrasonic disperse 30min, obtain CNTs dispersion liquid；
Step 2, weigh 3.8gNa3PO4·12H2O and 3.4gAgNO3, it is dissolved in 30mL distilled water respectively, by AgNO under magnetic stirring condition3Solution joins Na3PO4In solution, and continue magnetic stirring 10min at ambient temperature, form yellow suspension；
Step 3, yellow suspension step 2 configured join step 1) in the CNTs dispersion liquid of ultrasonic disperse that configures, after continuing ultrasonic disperse 30min, obtain precursor liquid, wherein CNTs and Ag3PO4Mass ratio be 1:10 1:30；
The pH value of the mixing precursor liquid that step 4, regulating step 3 obtain is to 3 12；
Step 5, the precursor liquid of step 4 is moved in stainless steel cauldron, be then placed in baking oven, under 120 DEG C of 180 DEG C of reaction temperatures, heat 4h 24h；
Step 6, after step 5 reaction terminates, be cooled to room temperature, filter reactant, in 60 DEG C of 80 DEG C of dry 4h after the solid distilled water wash of gained, then grind, obtain CNTs-Ag3PO4Photocatalyst。
The present invention proposes a kind of with the prepared CNTs-Ag of CNT material with carbon element3PO4Composite photo-catalyst and simple hydrothermal synthesis method thereof。
CNTs-Ag3PO4The Photocatalytic Degradation Property of catalysis material is to be characterized by sunlight color dysprosium lamp photo-catalytic degradation of methyl-orange (MO) solution。Specific experiment process is as follows: by the CNTs-Ag of 0.3g3PO4Photocatalyst is scattered in the methyl orange solution of 20mg/L, and Photoreactor is placed in the dark place 30min adsorption-desorption balance to reach between catalyst and dye molecule。At ambient temperature, irradiating with sunlight color dysprosium lamp, take 4mL sample every 20min, after 0.22 μm of water system filter filters, ultraviolet-uisible spectrophotometer measures filtrate absorbance in 462nm place。CNTs-Ag3PO4Photocatalyst for the photocatalytic degradation of methyl orange within the scope of experimental concentration linear, obey First-order kinetics equation: lnC0/ Ct=kt, therefore, can evaluate the photocatalysis performance of catalysis material with degradation rate constant k。
CNTs-Ag3PO4The structure characterization methods of catalysis material: by the crystal structure of X-ray diffraction (XRD) spectrum analysis sample and crystallization situation, with BET characterization test sample specific surface area, by the light absorbing state of ultraviolet spectrometer analysis of material。
The beneficial effects of the present invention is: the invention provides a kind of preparation method, the material with carbon element-Ag that it is carrier with material with carbon element that Hydrothermal Synthesis is prepared for3PO4Photocatalyst, prepared synthetic catalyst shows efficient Photocatalytic Degradation Property, and this provides certain theoretical basis and application directs for the novel Treatment process developing poisonous, harmful organic dyestuff in environmental improvement。The present invention have simple to operate, equipment requirements is low, without expensive reaction unit, the advantage being prone to high-volume synthesis etc., be expected to produce good Social and economic benef@。
Accompanying drawing explanation
Fig. 1 is CNTs and Ag in embodiment 13PO4The CNTs-Ag that mass ratio is 1:213PO4Different hydrothermal temperatures under XRD figure spectrum, the CNTs-Ag of other ratio3PO4Similar to it。
Fig. 2 is CNTs and Ag in embodiment 13PO4The CNTs-Ag that mass ratio is 1:213PO4Different pH under XRD figure spectrum, the CNTs-Ag of other ratio3PO4Similar to it。
Fig. 3 is CNTs and Ag in embodiment 13PO4The CNTs-Ag that mass ratio is 1:213PO4UV-Vis DRS (UV-visDRS)。
Fig. 4 is CNTs and Ag in embodiment 13PO4The Ag that mass ratio is 1:213PO4Pattern SEM figure, the CNTs-Ag of other ratio of photocatalyst3PO4Similar to it, that Fig. 4 (a) is Fig. 4 (b) partial enlarged drawing。
Fig. 5 is CNTs and Ag in embodiment 13PO4The CNTs-Ag that mass ratio is 1:213PO4Pattern SEM figure, the CNTs-Ag of other ratio of photocatalyst3PO4Similar to it, that Fig. 5 (a) is Fig. 5 (b) partial enlarged drawing。
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be further described in detail, but this explanation will not be construed as limiting the invention。
Embodiment 1:
CNTs-Ag3PO4The preparation process of catalysis material is as follows:
1) CNT (CNTs) weighing certain mass is put in the beaker filling 30mL distilled water, after ultrasonic disperse 30min, obtains CNTs dispersion liquid；
2) 3.8gNa is weighed3PO4·12H2O and 3.4gAgNO3, it is dissolved in 30mL distilled water respectively, by AgNO under magnetic stirring condition3Solution joins Na3PO4In solution, and continue magnetic stirring 10min at ambient temperature, form yellow suspension；
3) by step 2) yellow suspension that configures joins step 1) in the CNTs dispersion liquid of ultrasonic disperse that configures, after continuing ultrasonic disperse 30min, obtain precursor liquid, wherein CNTs and Ag3PO4Mass ratio be 1:10 1:30 (concrete mass ratio respectively 1:10,1:15,1:20,1:25,1:30)；
4) with nitric acid regulating step 3) the mixing precursor liquid pH value that obtains is 3 12 (concrete pH is 3.68,7.21,8.68,10.05 and 11.89 respectively)。
5) by step 4) it is transferred in the precursor liquid immigration stainless steel cauldron of certain pH value, be then placed in baking oven, heat under 120 DEG C 180 DEG C (actual temp is 120 DEG C, 140 DEG C, 160 DEG C, 180 DEG C respectively) reaction temperatures certain time 4h 24h (respectively 4h of concrete time, 8h, 12h, 18h, 24h)。
6) until step 5) after reaction terminates, be cooled to room temperature, filter reactant, the solid of gained with after distilled water wash 5 times in 60 DEG C of baking ovens dry 4h, then grind, obtain CNTs-Ag3PO4Photocatalyst。
Fig. 1 is CNTs-Ag3PO4Different hydrothermal temperatures under XRD figure spectrum, from CNTs-Ag3PO4XRD figure in it can be seen that the addition of CNTs does not change Ag3PO4Characteristic peak, illustrate that CNTs is not introduced into Ag3PO4In lattice。It addition, CNTs-Ag3PO4The characteristic peak (it is 26.0 ° and 43.3 ° that peak position is set to 2 θ) of CNTs do not occur in the XRD figure spectrum of photocatalyst, this is possibly due to the degree of crystallinity of CNTs well below Ag3PO4Degree of crystallinity, cause that the peak height of CNTs is by Ag3PO4Hide。
Fig. 2 is CNTs-Ag3PO4Different pH under XRD figure spectrum, when hydro-thermal precursor liquid is acid condition, CNTs-Ag3PO4Photocatalyst all go out peak position and Ag3PO4Diffraction maximum position in normal data JPCDS (06-0505) is consistent, and CNTs-Ag3PO4Peak type is sharp-pointed, and cutting edge of a knife or a sword is stronger, it does not have impurity peaks occurs, illustrates that the CNTs-Ag3PO4 photocatalyst purity of preparation is higher when precursor liquid pH is 3.68, has good degree of crystallinity。And when precursor liquid is neutral to time under alkali condition, although the peak type of Ag3PO4 characteristic peak, cutting edge of a knife or a sword are by force compared with acid condition, there is not significant change, but it is but that 38.1 °, 44.2 °, 64.3 °, 77.3 ° positions impurity peaks occur at 2 θ, the normal data JPCDS (04-0783) of these four diffraction maximums and Ag matches, this illustrates have simple substance Ag to generate in CNTs-Ag3PO4 photocatalyst, and the diffraction maximum of Ag is along with the increase of precursor liquid pH, peak type is more sharp-pointed, cutting edge of a knife or a sword becomes by force strong, and crystallization degree is more and more higher。
Fig. 3 is CNTs-Ag3PO4UV-Vis DRS (UV-visDRS), as seen from the figure, CNTs-Ag3PO4Spectral absorption scope relatively wide, in visible region, have stronger absorption。
Fig. 4 is Ag3PO4The pattern SEM figure of photocatalyst, it can be seen that Ag3PO4Being mostly irregular ball-type and some polyhedrals, dispersion ratio is more uniform。
Fig. 5 is CNTs-Ag3PO4The pattern SEM figure of photocatalyst, by scheming it can be seen that after adding CNTs, Ag3PO4Pattern be substantially free of and change, CNTs is close around at Ag3PO4Around。
The Ag by BET characterization test3PO4And CNTs-Ag3PO4Specific surface area。It is shown that Ag3PO4Specific surface area be 0.11m2/ g, CNTs-Ag3PO4Specific surface area be 6.72m2/ g。Visible, by compound CNTs, by means of the high-specific surface area of CNTs, improve the specific surface area of catalyst, this is for improving CNTs-Ag3PO4Catalysis activity have certain help。
Embodiment 2:
In order to check precursor liquid pH value to CNTs-Ag3PO4The impact of visible light activity, except precursor liquid pH value, other reaction condition such as hydrothermal temperature is 160 DEG C, the hydro-thermal time is 8h, CNTs and Ag3PO4Mass ratio be that 1:20, baking temperature 60 DEG C etc. are all identical with embodiment 1。It is shown that when precursor liquid pH value is 3.68, CNTs-Ag3PO4Total percent of decolourization of methyl orange is the highest, and the catalyst of preparation when precursor liquid pH is neutral meta-alkalescence, decolorizing effect takes second place, and when precursor liquid pH is original 11.89, decolorizing effect is poor。When precursor liquid pH is 3.68, total percent of decolourization of methyl orange is 99.7% by CNTs-Ag3PO4；When precursor liquid pH is 7.21, total percent of decolourization of methyl orange is 98.1% by CNTs-Ag3PO4；When precursor liquid pH is 8.68, total percent of decolourization of methyl orange is 97.8% by CNTs-Ag3PO4；When precursor liquid pH is 10.05, total percent of decolourization of methyl orange is 97.7% by CNTs-Ag3PO4；When precursor liquid pH is 11.89, total percent of decolourization of methyl orange is 93.9% by CNTs-Ag3PO4。In general, CNTs-Ag3PO4Decoloring ability strengthen gradually along with the reduction of synthetic catalyst precursor liquid pH value。Therefore, at CNTs-Ag3PO4In the preparation process of photocatalyst, best precursor liquid pH value is 3.68。
Embodiment 3:
In order to check hydrothermal temperature to CNTs-Ag3PO4The impact of visible light activity, except hydrothermal temperature, other reaction conditions such as precursor liquid pH is 3.68, the hydro-thermal time is 8h, CNTs and Ag3PO4Mass ratio be that 1:20, baking temperature 60 DEG C etc. are all identical with embodiment 1。When hydrothermal temperature is 120 DEG C, total percent of decolourization of methyl orange is 97.3% by CNTs-Ag3PO4；When hydrothermal temperature is 140 DEG C, total percent of decolourization of methyl orange is 94.2% by CNTs-Ag3PO4；When hydrothermal temperature is 160 DEG C, total percent of decolourization of methyl orange is 99.7% by CNTs-Ag3PO4；When hydrothermal temperature is 180 DEG C, total percent of decolourization of methyl orange is 95.8% by CNTs-Ag3PO4。It is shown that when hydrothermal temperature is 160 DEG C, the percent of decolourization of methyl orange is the highest。This result should be relevant with its degree of crystallinity and particle diameter。Catalyst crystal degree is more good, and light induced electron-hole is less susceptible to compound；Particle diameter is more little, and the time that electronics is diffused into surface from catalytic inner on the one hand is also more short, and electronics is also more little with hole-recombination probability, and specific surface area is also more big on the other hand, and photocatalytic activity position is more many, and catalyst activity is more high。Therefore, at CNTs-Ag3PO4In the preparation process of photocatalyst, best hydrothermal temperature is 160 DEG C。
Embodiment 4:
In order to check the hydro-thermal time to CNTs-Ag3PO4The impact of activity, dewaters outside the heat time, and other reaction condition such as precursor liquid pH is 3.68, hydrothermal temperature is 160 DEG C, CNTs and Ag3PO4Mass ratio be that 1:20, baking temperature 60 DEG C etc. are all identical with embodiment 1。The CNTs-Ag3PO4 of hydro-thermal reaction 8h, through photoreaction 30min, solution can be made to decolour, and hydro-thermal reaction 24h takes second place, after photoreaction 45min, can substantially remove methyl orange, and the photocatalyst visible light activity prepared without hydro-thermal reaction is more weak, light degradation speed is significantly slower, more than photoreaction 75min, reaction can be only achieved balance, and the clearance to methyl orange is about 88%。It is shown that when the hydro-thermal time is 8h, CNTs-Ag3PO4The light degradation speed of methyl orange is the fastest。The hydro-thermal time is to CNTs-Ag3PO4The impact of visible light activity does not have certain rule to follow, but in general, when being 4h without hydro-thermal reaction or hydro-thermal reaction time, the activity of catalyst is relatively low, and it is shorter that this is possibly due to generated time, and catalyst crystal degree is bad。Therefore, at CNTs-Ag3PO4In the preparation process of photocatalyst, the best hydro-thermal time is about 8h。
Embodiment 5:
In order to check CNTs-Ag3PO4Ag compared by synthetic catalyst3PO4The catalyst impact on visible light activity, in addition to be not added with outside people CNTs, remaining reaction condition such as precursor liquid pH is 3.68, hydrothermal temperature is 160 DEG C, the hydro-thermal time is that 8h, baking temperature 60 DEG C etc. are all identical with embodiment 1。Ag3PO4 photocatalyst is after illumination 30min, and reaction reaches balance, and CNTs-Ag3PO4 photocatalyst only light requirement, according to 20min, can make solution decolour。It is shown that CNTs-Ag3PO4With Ag3PO4Under visible light illumination, stronger photocatalytic degradation capability, CNTs-Ag are all shown3PO4The degradation rate of Visible Light Induced Photocatalytic methyl orange more quick, reaction rate is Ag3PO4Twice。Therefore, the addition of CNTs, the ratio of CNTs and Ag3PO4 is 1:20, it is possible to rate of photocatalytic oxidation is improved。
Claims (3)
1. a CNT-Ag3PO4Composite catalyst, is characterized in that: it is by the aqueous dispersions of CNT (CNTs) and Ag3PO4Aqueous suspension mix homogeneously, at 120 DEG C-180 DEG C CNT-Ag obtained for hydro-thermal 4-24 hour3PO4Composite catalyst。
2. composite catalyst according to claim 1, is characterized in that: described CNT and Ag3PO4Mass ratio is 1:10 1:30。
3. the CNTs-Ag described in a claim 1 or 23PO4The preparation method of catalyst, it is characterised in that comprise the following steps:
Step 1, the CNTs weighing certain mass are put in the beaker filling 30mL distilled water, after ultrasonic disperse 30min, obtain CNTs dispersion liquid；
Step 2, weigh 3.8gNa3PO4·12H2O and 3.4gAgNO3, it is dissolved in 30mL distilled water respectively, by AgNO under magnetic stirring condition3Solution joins Na3PO4In solution, and continue magnetic stirring 10min at ambient temperature, form yellow suspension；
Step 3, yellow suspension step 2 configured join step 1) in the CNTs dispersion liquid of ultrasonic disperse that configures, after continuing ultrasonic disperse 30min, obtain precursor liquid, wherein CNTs and Ag3PO4Mass ratio be 1:10 1:30；
The pH value of the mixing precursor liquid that step 4, regulating step 3 obtain is to 3 12；
Step 5, the precursor liquid of step 4 is moved in stainless steel cauldron, be then placed in baking oven, under 120 DEG C of 180 DEG C of reaction temperatures, heat 4h 24h；
Step 6, after step 5 reaction terminates, be cooled to room temperature, filter reactant, in 60 DEG C of 80 DEG C of dry 4h after the solid distilled water wash of gained, then grind, obtain CNTs-Ag3PO4Photocatalyst。
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| CN106807428A (en) * | 2017-02-20 | 2017-06-09 | 南京大学 | C with visible light catalysis activity3N4‑BiVO4Catalyst and preparation method thereof |
| CN106807414A (en) * | 2017-01-06 | 2017-06-09 | 华南理工大学 | A kind of silver orthophosphate/bromination silver/carbon nanotube composite photo-catalyst and preparation and application |
| CN107029777A (en) * | 2017-05-26 | 2017-08-11 | 长沙学院 | Composite visible light catalyst and its preparation method and application |
| CN108906093A (en) * | 2018-06-07 | 2018-11-30 | 湖南大学 | A kind of preparation method using carbon nanotube control silver orthophosphate crystal particle diameter |
| CN109499591A (en) * | 2018-11-15 | 2019-03-22 | 江苏大学 | It is a kind of can magnetic recovery class light fenton catalyst preparation method and applications |
| CN109621993A (en) * | 2019-01-15 | 2019-04-16 | 湖南大学 | Utilize silver orthophosphate/multi-walled carbon nanotube/bismuth tungstate composite photocatalyst material processing antibiotic method |
| CN109621994A (en) * | 2019-01-15 | 2019-04-16 | 湖南大学 | Silver orthophosphate/multi-walled carbon nanotube/bismuth tungstate composite photocatalyst material and preparation method thereof |
| CN113797943A (en) * | 2021-10-03 | 2021-12-17 | 桂林理工大学 | Preparation method of composite photocatalyst with carbon nano tube as carrier |
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| CN106732790A (en) * | 2016-12-02 | 2017-05-31 | 东华大学 | A kind of fiber/CNT/Ag3PO4 three-dimensional recyclable efficient catalytic material and its preparation and application |
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| CN108906093A (en) * | 2018-06-07 | 2018-11-30 | 湖南大学 | A kind of preparation method using carbon nanotube control silver orthophosphate crystal particle diameter |
| CN109499591A (en) * | 2018-11-15 | 2019-03-22 | 江苏大学 | It is a kind of can magnetic recovery class light fenton catalyst preparation method and applications |
| CN109499591B (en) * | 2018-11-15 | 2021-02-12 | 江苏大学 | Preparation method and application of magnetically-recoverable photo-Fenton-like catalyst |
| CN109621993A (en) * | 2019-01-15 | 2019-04-16 | 湖南大学 | Utilize silver orthophosphate/multi-walled carbon nanotube/bismuth tungstate composite photocatalyst material processing antibiotic method |
| CN109621994A (en) * | 2019-01-15 | 2019-04-16 | 湖南大学 | Silver orthophosphate/multi-walled carbon nanotube/bismuth tungstate composite photocatalyst material and preparation method thereof |
| CN113797943A (en) * | 2021-10-03 | 2021-12-17 | 桂林理工大学 | Preparation method of composite photocatalyst with carbon nano tube as carrier |
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Application publication date: 20160622 |