CN105233846A - Preparation method and application of SnO2/Ag3PO4 composite photocatalyst - Google Patents

Preparation method and application of SnO2/Ag3PO4 composite photocatalyst Download PDF

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CN105233846A
CN105233846A CN201510718937.7A CN201510718937A CN105233846A CN 105233846 A CN105233846 A CN 105233846A CN 201510718937 A CN201510718937 A CN 201510718937A CN 105233846 A CN105233846 A CN 105233846A
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catalyst
sno
composite photo
preparation
reaction
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逯子扬
黄海
闫永胜
宋旼珊
赵晓旭
高乃玲
马中飞
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Jiangsu University
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Jiangsu University
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Abstract

The invention provides a preparation method and an application of a SnO2/Ag3PO4 composite photocatalyst. According to the invention, sodium pyrophosphate is weighed and completely dissolved in distilled water, such that a solution A is obtained; a silver nitrate solution is slowly dropped into the obtained solution A, and a mixed liquid B is obtained when dropping is finished; the mixed liquid B is subjected to a reaction under stirring; after the reaction, a potassium stannate solution is slowly dropped into the mixed liquid B; the mixture is well mixed by stirring, such that a mixed liquid C is obtained; the mixed liquid C is transferred into a hydrothermal reaction kettle, and is subjected to a thermostatic thermal reaction; when the reaction is finished, the reaction kettle is cooled to room temperature; and a product is subjected to centrifugation separation, washing and drying, such that the SnO2/Ag3PO4 composite photocatalyst is obtained. The SnO2/Ag3PO4 composite photocatalyst provided by the invention has good morphology and photocatalytic activity. With the loading of SnO2, Ag3PO4 photo-generated electron transfer is effectively improved, and Ag3PO4 impedance and photocurrent are ameliorated, such that Ag3PO4 photo-corrosion effect is inhibited, and stability is greatly improved.

Description

A kind of SnO 2/ Ag 3pO 4the Preparation method and use of composite photo-catalyst
Technical field
The invention belongs to technical field of environmental material preparation, be specifically related to the SnO that an a kind of step hydro-thermal preparation has high stability 2/ Ag 3pO 4the method of composite photo-catalyst.
Background technology
Silver orthophosphate (Ag 3pO 4) show very strong oxidability under light illumination as a kind of novel photochemical catalyst, there is very strong degradation to the organic pollution in solution, Ag 3pO 4well can absorb the sunshine of 420nm ~ 520nm, show up to 90% quantum yield, this parameter is better than general photochemical catalyst.Ag 3pO 4energy gap be 2.36eV, can be good at utilizing sunshine.Decomposable asymmetric choice net organic dyestuff under the irradiation of visible ray, and its oxidation activity is the decades of times of existing photochemical catalyst.But Ag 3pO 4under light illumination, easily with the electron reaction produced, extremely unstable, this seriously constrains Ag 3pO 4application and development.
Tin ash (SnO 2) be a kind of electric conductivity and stability all well material, with Ag 3pO 4the transfer of light induced electron can be promoted after compound, improve the separative efficiency in electronics and hole, and then strengthen its active and stability.And SnO 2good permeability is had to sunshine, with Ag as transparent material 3pO 4compound does not affect its absorption to light.
Therefore, the present invention selects sodium pyrophosphate, silver nitrate and potassium stannate to be presoma, prepares SnO by one step hydro thermal method 2/ Ag 3pO 4composite photo-catalyst, simplifies the preparation process of photochemical catalyst, avoids the introducing of impurity simultaneously.Prepared SnO 2/ Ag 3pO 4composite photo-catalyst not only has good pattern and photocatalytic activity, also has higher stability.
Summary of the invention
The present invention has prepared SnO with one step hydro thermal method 2/ Ag 3pO 4composite photo-catalyst.Its advantage is prepared SnO 2/ Ag 3pO 4composite photo-catalyst not only has higher photocatalytic activity but also have good stability.
The technical solution used in the present invention is:
An a kind of step hydro-thermal preparation has the SnO of high stability 2/ Ag 3pO 4the method of composite photo-catalyst, carry out according to following step:
Step 1, take sodium pyrophosphate and be dissolved in distilled water, dissolve completely, obtain solution A;
Slowly drip liquor argenti nitratis ophthalmicus in step 2, the solution A that obtains to step 1, after dropwising, be obtained by reacting mixed liquid B under agitation;
Slowly drip potassium stannate solution in step 3, mixed liquid B in step 2, obtain mixed liquor C after stirring, mixed liquor C is transferred in hydrothermal reaction kettle and carries out constant temp. heating reaction, after reaction terminates, reactor is cooled to room temperature, then by product centrifugation, washing, drying, obtains SnO 2/ Ag 3pO 4composite photo-catalyst.
In described step 1, the amount ratio of sodium pyrophosphate and distilled water is 1.5g:25mL.
In described step 2, described liquor argenti nitratis ophthalmicus concentration is 0.2M, and added liquor argenti nitratis ophthalmicus and the volume ratio of solution A are 9:25.
In described step 2, the time of stirring reaction is 1h.
In described step 3, the concentration of described potassium stannate solution is 0.2M, and added potassium stannate solution and the volume ratio of mixed liquid B are 1 ~ 3:340, is preferably 1:170.
In described step 3, the temperature of described constant temp. heating reaction is 120 ~ 160 DEG C, and the reaction time is 12h.
In described step 3, the temperature of described constant temp. heating reaction is preferably 140 DEG C.
Described SnO 2/ Ag 3pO 4composite photo-catalyst is used for photocatalytic degradation tetracycline.
Technological merit of the present invention:
(1) SnO in the present invention 2/ Ag 3pO 4composite photo-catalyst has good pattern and photocatalytic activity.
(2) pure Ag 3pO 4, photoetch effect can be there is when illumination in less stable, and SnO in the present invention 2load effectively raise Ag 3pO 4the transfer of light induced electron, improve Ag 3pO 4impedance and photoelectric current, thus inhibit Ag 3pO 4photoetch effect, drastically increase stability.
Accompanying drawing explanation
Fig. 1: be the SnO prepared under different hydrothermal temperature 2/ Ag 3pO 4the SEM figure of composite photo-catalyst, wherein a and b is 120 DEG C; C and d is 140 DEG C; E and f is 160 DEG C;
Fig. 2: for different hydrothermal temperature is to SnO 2/ Ag 3pO 4the impact of the photocatalytic activity of composite photo-catalyst, wherein a is 120 DEG C; B is 140 DEG C; C is 160 DEG C;
Fig. 3: be different Ag 3pO 4with SnO 2the SnO of mol ratio 2/ Ag 3pO 4the SEM figure of composite photo-catalyst and EDS spectrogram, wherein a is 30:1; B is 15:1; C is 10:1;
Fig. 4: be the UV-Vis DRS spectrogram of different photochemical catalyst;
Fig. 5: be the photocatalytic activity figure of different photochemical catalyst, wherein a is Ag 3pO 4; B is the SnO of 30:1 2/ Ag 3pO 4composite photo-catalyst; C is the SnO of 15:1 2/ Ag 3pO 4composite photo-catalyst; D is the SnO of 10:1 2/ Ag 3pO 4composite photo-catalyst; E is SnO 2;
Fig. 6: be Ag 3pO 4and SnO 2/ Ag 3pO 45 circulation light catalytic effect figure of composite photocatalyst for degrading tetracycline;
Fig. 7: be the XRD spectra of different photochemical catalyst;
Fig. 8: be SnO 2/ Ag 3pO 4the XPS spectrum figure of composite photo-catalyst, wherein a is score; B is Ag3d; C is P2p; D is O1s; E is Sn3d;
Fig. 9: be Ag 3pO 4and SnO 2/ Ag 3pO 4the electrochemical impedance spectrogram of composite photo-catalyst;
Figure 10: be Ag 3pO 4and SnO 2/ Ag 3pO 4the photocurrent response figure of composite photo-catalyst.
Detailed description of the invention
Below in conjunction with concrete embodiment, the present invention will be further described.
Photocatalytic activity evaluation: carry out in D1 type photochemical reaction instrument (purchased from Educational Instrument Factory of Yangzhou University), the tetracycline simulated wastewater of 50mL20mg/L is added in reaction bulb, add the photochemical catalyst prepared by magneton and 0.02g again, open visible ray power supply and aerator, starting external thermostatic water-circulator bath control temperature of reaction system is 30 DEG C.Dynamic Adsorption, carries out illumination reaction after arriving adsorption equilibrium, and every sampling in 10 minutes once, centrifugation, surveys the concentration of tetracycline in supernatant, pass through C/C 0judge antibiotic degradation effect.Wherein, C 0for the concentration of tetracycline after adsorption equilibrium, the concentration of tetracycline when C is reaction time T.
Embodiment 1:
(1) SnO 2/ Ag 3pO 4composite photo-catalyst: take 1.5g sodium pyrophosphate and be dissolved in 25mL distilled water, slowly dripping the liquor argenti nitratis ophthalmicus of 9mL0.2mol/L after dissolving completely, in solution, generate white precipitate rapidly, stirring 1h to reacting completely, slowly drip 0.2mL0.2mol/L potassium stannate solution again, be transferred in hydrothermal reaction kettle after continuing to stir 30min, at 140 DEG C, react 12h, after reaction terminates, reactor is cooled to room temperature, then by above-mentioned sample centrifugation, after washing three times with distilled water, dry, SnO 2/ Ag 3pO 4composite photo-catalyst (wherein Ag 3pO 4with SnO 2molar ratio be 15:1).
(2) get sample in 0.02g (1) and carry out photocatalytic degradation test in photochemical reaction instrument, experimental result ultraviolet specrophotometer analysis, records this SnO 2/ Ag 3pO 4composite photo-catalyst is very good to the light degradation effect of tetracycline, shows this SnO 2/ Ag 3pO 4composite photo-catalyst has stronger photocatalytic activity.
Embodiment 2:
Undertaken by the same step of embodiment 1 preparation technology, unlike hydrothermal temperature in step (1) get three groups of different temperatures 120 DEG C, 140 DEG C, 160 DEG C, prepare different SnO 2/ Ag 3pO 4composite photo-catalyst, investigates different hydrothermal temperature to SnO 2/ Ag 3pO 4the impact of composite photo-catalyst crystal structure, as shown in Figure 1, as can be seen from the figure the sample particle that obtains of 120 DEG C of hydro-thermal reaction 12h is less, and be about 400nm, pattern is mixed and disorderly for result.And temperature when being upgraded to 140 DEG C prepared composite photo-catalyst there is the crystal structure of comparatively rule, be typical Ag 3pO 4, and when temperature is 160 DEG C, the composite photo-catalyst particle diameter of formation again increases and pattern also becomes random state.As can be seen from Figure 2 when hydrothermal temperature is 140 DEG C, prepared SnO 2/ Ag 3pO 4composite photo-catalyst has best Photocatalytic activity, be secondly 160 DEG C, and 120 DEG C the poorest.In sum, in this application by SnO prepared by one step hydro thermal method 2/ Ag 3pO 4the optimum temperature of composite photo-catalyst is 140 DEG C, SnO prepared by this temperature 2/ Ag 3pO 4composite photo-catalyst not only pattern is better, and activity is also the highest simultaneously.
Embodiment 3:
Undertaken by the same step of embodiment 1 preparation technology, measure 0.1mL, 0.2mL and 0.3mL unlike adding of potassium stannate in step (1), namely the mol ratio of silver nitrate and potassium stannate is that 30:1,15:1,10:1 are to prepare the SnO of different mol ratio 2/ Ag 3pO 4composite photo-catalyst, investigates different mol ratio to SnO 2/ Ag 3pO 4the impact of composite photo-catalyst pattern, result as shown in Figure 3, as can be seen from Figure 3 Ag 3pO 4and SnO 2snO prepared when mol ratio is 30:1 2/ Ag 3pO 4the pattern of composite photo-catalyst is comparatively homogeneous, and only there is a small amount of SnO on its surface 2load.When the mol ratio improving potassium stannate solution is 15:1, the SnO of good pattern and proterties can be formed 2/ Ag 3pO 4composite photo-catalyst.Continuing to improve rate of charge is 10:1, forms random pattern composite photo-catalyst.As can be seen from Figure 4 SnO 2/ Ag 3pO 4composite photo-catalyst has and comparatively significantly increases being less than absorption intensity within the scope of 525nm, and along with SnO 2the increase of ratio, it is to the absorption intensity of light also corresponding increase, and this shows SnO 2compound can improve absorption to light.As can be seen from Figure 5 simple SnO 2substantially degrading activity is not had to tetracycline, simple Ag 3pO 4not high to tetracycline degradation efficiency yet.And different Ag 3pO 4with SnO 2the SnO of mol ratio 2/ Ag 3pO 4composite photo-catalyst has different effects, and wherein ratio is two kinds of SnO of 30:1 and 15:1 2/ Ag 3pO 4the activity of composite photo-catalyst is better than simple Ag 3pO 4, and ratio is the SnO of 10:1 2/ Ag 3pO 4the photocatalytic activity of composite photo-catalyst is not as simple Ag 3pO 4.To sum up Ag is described 3pO 4with SnO 2snO when mol ratio is 15:1 2/ Ag 3pO 4composite photo-catalyst has good photocatalytic activity and pattern.
Embodiment 4:
SnO is investigated by (2) step in embodiment 1 2/ Ag 3pO 4the photochemical stability of composite photo-catalyst photocatalytic degradation tetracycline, result as shown in Figure 6, as can be seen from the figure 5 times circulation after, SnO 2/ Ag 3pO 4the change of the photocatalysis efficiency of composite photo-catalyst is very little, and simple Ag 3pO 4after 5 circulations, its photocatalysis efficiency obviously reduces, the SnO prepared by explanation 2/ Ag 3pO 4composite photo-catalyst has good photochemical stability and reusing.
As can be seen from Figure 7 prepared Ag 3pO 4there is comparatively significantly crystal structure.Show by the good Ag of crystal structure can be prepared to the hydrothermal treatment consists of pyrophosphoric acid 3pO 4.Simultaneously with potassium stannate for presoma is by the SnO prepared by hydro-thermal method 2obvious characteristic peak is shown 26.6 °, 33.9 ° and 51.8 °.From pressing different Ag 3pO 4with SnO 2snO prepared by molar ratio 2/ Ag 3pO 4in the XRD diffraction spectrogram of composite photo-catalyst, clearly can find Ag 3pO 4and SnO 2characteristic peak, this shows SnO in water-heat process 2can load smoothly at Ag 3pO 4surface, and the integrality maintaining the two crystal structure.As can be seen from figure also, along with Ag 3pO 4with SnO 2the change of molar ratio, prepared SnO 2/ Ag 3pO 4snO in the XRD diffraction spectrogram of composite photo-catalyst 2characteristic peak intensity also along with change.
Prepared SnO can be found out from Fig. 8 a 2/ Ag 3pO 4containing Ag, P, O and Sn element in composite photo-catalyst.Fig. 8 b is the high-resolution spectrogram of Ag3d, and two peaks being wherein positioned at 374eV and 367.8eV are Ag3d 3/2and Ag3d 5/2characteristic peak.Fig. 8 c is the high-resolution spectrogram of P2p, and wherein the peak of 132.6eV is PO 4 3-the characteristic peak of middle P element.In Fig. 8 d, 530.4eV place is Ag 3pO 4and SnO 2the characteristic peak of middle O element.Fig. 8 e is the high-resolution spectrogram of Sn3d, Sn3d as we can see from the figure 3/2and Sn3d 4/2be positioned at the characteristic peak of 495.4eV and 486.8eV, it is SnO that the above results demonstrates obtained photochemical catalyst 2/ Ag 3pO 4composite photo-catalyst.
As can be seen from Figure 9 SnO under visible light illumination 2/ Ag 3pO 4electrochemical impedance spectroscopy half circular diameter of composite photo-catalyst is significantly less than Ag 3pO 4.SnO is described 2load effectively raise material conductivity, simultaneously also show SnO 2load to Ag 3pO 4when illumination, the transfer of electronics and the separation of electron hole have obvious effect.
As can be seen from Figure 10 SnO 2/ Ag 3pO 4composite photo-catalyst photoelectric current has had obvious lifting, and this is the SnO due to high conductivity 2transferable light induced electron, restrained effectively the compound in electronics and hole.This shows, SnO in the application 2/ Ag 3pO 4composite photo-catalyst will produce the degraded that more active material is conducive to object.

Claims (9)

1. a SnO 2/ Ag 3pO 4the preparation method of composite photo-catalyst, is characterized in that, carries out according to following step:
Step 1, take sodium pyrophosphate and be dissolved in distilled water, dissolve completely, obtain solution A;
Slowly drip liquor argenti nitratis ophthalmicus in step 2, the solution A that obtains to step 1, after dropwising, be obtained by reacting mixed liquid B under agitation;
Slowly drip potassium stannate solution in step 3, mixed liquid B in step 2, obtain mixed liquor C after stirring, mixed liquor C is transferred in hydrothermal reaction kettle and carries out constant temp. heating reaction, after reaction terminates, reactor is cooled to room temperature, then by product centrifugation, washing, drying, obtains SnO 2/ Ag 3pO 4composite photo-catalyst.
2. a kind of SnO according to claim 1 2/ Ag 3pO 4the preparation method of composite photo-catalyst, is characterized in that, in step 1, the amount ratio of sodium pyrophosphate and distilled water is 1.5g:25mL.
3. a kind of SnO according to claim 1 2/ Ag 3pO 4the preparation method of composite photo-catalyst, is characterized in that, in step 2, described liquor argenti nitratis ophthalmicus concentration is 0.2M, and added liquor argenti nitratis ophthalmicus and the volume ratio of solution A are 9:25.
4. a kind of SnO according to claim 1 2/ Ag 3pO 4the preparation method of composite photo-catalyst, is characterized in that, in step 2, the time of stirring reaction is 1h.
5. a kind of SnO according to claim 1 2/ Ag 3pO 4the preparation method of composite photo-catalyst, is characterized in that, in step 3, the concentration of described potassium stannate solution is 0.2M, and added potassium stannate solution and the volume ratio of mixed liquid B are 1 ~ 3:340.
6. a kind of SnO according to claim 5 2/ Ag 3pO 4the preparation method of composite photo-catalyst, is characterized in that, added potassium stannate solution and the volume ratio of mixed liquid B are 1:170.
7. a kind of SnO according to claim 1 2/ Ag 3pO 4the preparation method of composite photo-catalyst, is characterized in that, in step 3, the temperature of described constant temp. heating reaction is 120 ~ 160 DEG C, and the reaction time is 12h.
8. a kind of SnO according to claim 7 2/ Ag 3pO 4the preparation method of composite photo-catalyst, is characterized in that, the temperature of described constant temp. heating reaction is 140 DEG C.
9. the SnO described in claim 1 ~ 8 any one 2/ Ag 3pO 4the purposes of composite photo-catalyst, is characterized in that, described SnO 2/ Ag 3pO 4composite photo-catalyst is used for photocatalytic degradation tetracycline.
CN201510718937.7A 2015-10-28 2015-10-28 Preparation method and application of SnO2/Ag3PO4 composite photocatalyst Pending CN105233846A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106693908A (en) * 2017-01-17 2017-05-24 河南理工大学 Preparation method and application of nano composite material capable of simultaneously recognizing and efficient degrading tetracycline
CN108043433A (en) * 2017-12-11 2018-05-18 湖北大学 One kind four aoxidizes three tin/silver orthophosphate composite material photocatalyst and preparation method thereof
CN110152696A (en) * 2018-02-08 2019-08-23 彭万喜 A kind of digester of microenvironment pollution control
CN112067666A (en) * 2020-08-13 2020-12-11 东北电力大学 Preparation method of silver phosphate doped tin dioxide gas sensor gas sensitive material

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JP2012228659A (en) * 2011-04-26 2012-11-22 Sharp Corp Water purification device
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JP2012228659A (en) * 2011-04-26 2012-11-22 Sharp Corp Water purification device
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106693908A (en) * 2017-01-17 2017-05-24 河南理工大学 Preparation method and application of nano composite material capable of simultaneously recognizing and efficient degrading tetracycline
CN106693908B (en) * 2017-01-17 2019-01-18 河南理工大学 The preparation method and application of the simultaneously nanocomposite of efficient degradation tetracycline can be identified simultaneously
CN108043433A (en) * 2017-12-11 2018-05-18 湖北大学 One kind four aoxidizes three tin/silver orthophosphate composite material photocatalyst and preparation method thereof
CN110152696A (en) * 2018-02-08 2019-08-23 彭万喜 A kind of digester of microenvironment pollution control
CN112067666A (en) * 2020-08-13 2020-12-11 东北电力大学 Preparation method of silver phosphate doped tin dioxide gas sensor gas sensitive material
CN112067666B (en) * 2020-08-13 2024-03-29 东北电力大学 Preparation method of silver phosphate doped tin dioxide gas sensor gas-sensitive material

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