CN105214690B - A kind of flower-shaped heterojunction structure micron ball photocatalyst of tree peony and its preparation and application - Google Patents
A kind of flower-shaped heterojunction structure micron ball photocatalyst of tree peony and its preparation and application Download PDFInfo
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- CN105214690B CN105214690B CN201510619254.6A CN201510619254A CN105214690B CN 105214690 B CN105214690 B CN 105214690B CN 201510619254 A CN201510619254 A CN 201510619254A CN 105214690 B CN105214690 B CN 105214690B
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Abstract
The invention provides a kind of flower-shaped heterojunction structure micron ball photocatalyst of tree peony, because different in width from inside to outside can be with matching so that catalyst has multiwave absorption to sunshine, so as to drastically increase its disposal efficiency to the dyestuff in contaminant water.The catalyst is prepared using hydro-thermal method and base exchange method：The flower-shaped Zn In S micron balls of tree peony with different specific surface areas have been prepared first with hydrothermal synthesis method；The Zn In S of surface region are transformed into Ag In S followed by base exchange method and keep its pattern constant, by controlling reaction regulation to obtain the heterogeneous photochemical catalyst of different extinction wave bands.Compared to traditional TiO2Or for single ternary photochemical catalyst, it is more than 100 m with the good efficiency of light energy utilization, specific surface area2/ g, has very high photodegradation rate in the case of usage amount very little；The inventive method is easy, and generated time is short, and degradation efficiency is high, with obvious superiority and practical value.
Description
Technical field
The invention belongs to micro-nano synthetic material field, and in particular to a kind of flower-shaped heterojunction structure micron ball photocatalysis of tree peony
Agent and its preparation and application.
Background technology
Environment and the energy are 21 century mankind's area and significant problem urgently to be resolved hurrily.Dyestuff in mankind's daily life very
It is multi-field to have application, the industry such as clothes, building, food and drink.However, because many dyestuffs are all non-natural, chemical industry conjunctions
Into, therefore be difficult by natural degradation.Statistics shows that the dyestuff for accounting for Gross World Product 15% is lost in dyeing course
Lose, this has become global problem.Although many technologies can handle contaminated water, mostly have cost it is high,
The shortcomings of efficiency is low, byproduct is more.
In recent years, because photocatalysis can make full use of solar energy, a kind of important practical purified water skill has been made
Art.In many photochemical catalysts, titanium dioxide (TiO2) due to low with photolytic activity, safety non-toxic, high chemical stability, cost
The features such as obtained extensive reference.Yet with TiO2Band gap it is relatively wide, the sunshine of ultraviolet band can only be absorbed, therefore
It strongly limit its practical application.Although some synthetic methods can overcome, for example, continuously adsorbed quantum dot by surface
It is coupled to TiO2Surface, but there is preparation technology complexity in these methods, equipment cost is high, and the shortcomings of time loss is long turns into
The bottleneck of industrialized production.On the other hand, ternary semiconductor is due to gap tunable, very high resistance to defective and high stable
Property, obtain the extensive concern of people.But the band gap of the ternary semiconductor of single structure is relatively fixed, it is impossible to sufficiently utilize
Sunshine, thus with multiband absorb photochemical catalyst prepare it is extremely urgent.
The content of the invention
In order to realize the broad absorption to sunshine, efficient photocatalytically degradating organic dye, the purpose of the present invention are realized
It is to provide a kind of flower-shaped heterojunction structure micron ball photocatalyst of tree peony.A kind of flower-shaped heterojunction structure micron ball photocatalyst of tree peony,
It is followed successively by the Ag-In-S outer layers of Zn-In-S cores, 20-200nm Zn-Ag-In-S intermediate layers and 10-50nm from inside to outside；It is first
The flower-shaped Zn-In-S core micron balls of hydrothermal growth process synthesis tree peony are first passed through, it is thickness 50nm or so nanometer sheet to make its surface
Self assembly stacks the similar petal layer structure to be formed, and inside is solid；Then partial cation exchange process is utilized, by Zn-In-
The Zn-In-S of S core micron ball surface regions is transformed into Ag-In-S, and it is Zn-Ag-In-S to have a transition zone in the middle of this two layers
Intermediate layer.
It is preferred that, the flower-shaped micron ball of tree peony of the heterojunction structure is the control for contrasting surface area and optical absorption band gap
Micron ball；The size of the micron ball is 0.5-10 μm, pattern is that petal stratiform, specific surface area are 100-150m2/g。
It is a further object of the present invention to provide a kind of preparation method and applications of heterojunction structure micron ball photocatalyst.
In order to realize the purpose of the present invention, the invention provides a kind of high efficiency photocatalyst with high specific surface area
Preparation scheme：
(1) preparation of Zn-In-S micron balls：
By hydrothermal growth process, it is 1 to control reactant zinc salt, indium salts, the amount mol ratio of sulphur source:(0.8-3.2):(4-8)；
Control the pH value of reaction solution between 0.5-3, reaction temperature is 100-180 DEG C, the reaction time is 2-8 hours, obtains different chis
The flower-shaped Zn-In-S micron balls of very little tree peony；Alternately washing, the centrifugation of product ethanol and deionized water, is then stored in ethanol
Or in deionized water；
(2) preparation of the heterogeneous microballoons of Zn-In-S/Ag-In-S：
Zn-In-S micron balls obtained by step (1) are dispersed in the mixed liquor of first alcohol and water, pass through partial cation
Exchange, control adds 0.2-5mmol AgNO3And control solution acid alkalinity pH value between 0.5-3, reaction temperature be 100-
180 DEG C, the reaction time is 2-8 hours, and control obtains the Ag-In-S layers of different-thickness；Product ethanol and deionized water alternating
Washing, centrifugation, are then stored in ethanol or deionized water.
Preferential, zinc salt is selected from one of analogs such as zinc sulfate, zinc nitrate, zinc acetate or zinc chloride；Indium salts are selected from sulphur
One of analogs such as sour indium, indium nitrate, indium acetate or inidum chloride, sulphur source is selected from thioacetamide, thiocarbamide or vulcanized sodium etc.
One of analog or composition；Indium salts and the mol ratio of zinc salt are between 0.8-2.5, and the scope of pH value is between 0.5-3, sulphur
The amount of the material in source is 4-8 times of the amount of zinc salt material.
Preferential, the preparation of described Zn-In-S micron balls and the heterogeneous microballoons of Zn-In-S/Ag-In-S is in polytetrafluoroethyl-ne
Synthesized in the stainless steel autoclave of alkene lining, reaction temperature is 100-180 DEG C, the reaction time is 2-8 hours.
Further preferential, the reaction temperature of cation exchange reaction is 120-160 DEG C, and the reaction time is 4-6 hours.
Meanwhile, the invention provides the application of heterogeneous type micron ball dyestuff in photocatalytic degradation contaminant water.Specifically
For the photochemical catalyst of different structure, component is added in the dye discoloration aqueous solution, then under natural light or tungsten halogen lamp
Irradiate to realize the light degradation to dyestuff.
The positive effect of the present invention is as follows：
(1) the flower-shaped micron ball light of simple tree peony of the hydro-thermal method synthesis with different specific surface areas of use of the invention is urged
Agent so that material has high absorption efficiency to ultraviolet band；
(2) photochemical catalyst of heterojunction structure is synthesized using base exchange method first, while keeping high specific surface area
With the strong absorption to visible light wave range, so as to sufficiently make use of sunshine；
(3) the flower-shaped heterojunction structure micron ball photocatalyst of the tree peony can be realized effectively to dyestuff in contaminant water using light
Degraded.
Brief description of the drawings：
Fig. 1：The scanning electron microscope image of the different-shape of ZIS/AIS micron balls, correspond to embodiment 1 to embodiment 4, it is seen that
The pattern of product is very uniform, and surface is assembled by substantial amounts of nanometer sheet；
Fig. 2：The x-ray photoelectron energy spectrum diagram of microballoon before and after ion exchange, Zn characteristic peak weakens after reaction, and occurs
Ag characteristic peak；
Fig. 3：The ultraviolet-visible of micron ball-near infrared absorption spectrum, as illustrated, with the difference of reaction condition, product
Absorption characteristic is significantly different, and the absorption spectra after reaction is wider, shows there is stronger absorption to visible ray, and this is conducive to abundant profit
High efficiency photocatalysis is realized with luminous energy.
Fig. 4：Micron ball surface apertures measurement data, the aperture for showing product is all between 3-10nm, to belong to mesoporous material
Material, fully can adsorb and accommodate substantial amounts of pollutant.
Fig. 5：Light degradation fluorescent dyes rhodamine B efficiency changes with time, as seen from the figure, with prolonging for light application time
Long, the fluorescence of dyestuff is gradually reduced, and explanation molecular structure is destroyed for this, decompose, and the degradation rate after degraded in 50 minutes reaches
99.5%.
Embodiment
Below in conjunction with the accompanying drawings and its present invention is discussed in detail in embodiment.
1st, chemicals
Zinc acetate, zinc chloride, zinc nitrate, indium acetate, inidum chloride, indium nitrate, vulcanized sodium, thiocarbamide, thioacetamide, nitric acid
Silver, is that analysis is pure, is provided by Chemical Reagent Co., Ltd., Sinopharm Group.
2nd, concrete operations are as follows
(1) preparation of the flower-shaped Zn-In-S micron balls of tree peony of different specific surface areas
The 20-40mL aqueous solution is configured, the wherein concentration of zinc salt is 0.025~0.05mol/L, the concentration 0.020- of indium salts
Its pH value is adjusted to 0.5-3 with hydrochloric acid, then added by 0.125mol/L, i.e. In and Zn mol ratio between 0.8~2.5
10mL contains 4~8mmol sulphur sources, and sulphur source is selected from thioacetamide, vulcanized sodium either thiocarbamide or the solution of their combination.
Mixed liquor is transferred in the stainless steel autoclave of teflon lined, is reacted 2-8 hours at 100-180 DEG C.Cool down reaction solution,
Centrifugation, adds excessive ethanol washing, and product is scattered to be preserved in ethanol.
(2) preparation of the ZIS/AIS microballoons of different band gap
The a certain amount of Zn-In-S micron balls prepared are dispersed in the mixed liquor of 20mL first alcohol and waters, it is preferred that described
ZIS amount be defined by that preferably can be dispersed in mixed liquor, the volume ratio of wherein first alcohol and water is preferably 1:5, magnetic agitation
It is lower add it is a certain amount of containing 0.2-5mmol silver nitrate solutiones, stir 10-40 minutes.Then mixed liquor is transferred to poly- four
In the stainless steel autoclave of PVF lining, 120-180 DEG C is reacted 3-8 hours.Product processing mode is ibid.
Embodiment is chosen below does specific explaination：
Embodiment 1：
(1) indium acetate of 1mmol zinc acetate and 2mmol is dissolved in 40mL water, be adjusted to its pH with hydrochloric acid
2.5；Then the solution that 10mL contains 4mmol thioacetamides and 2mmol thiocarbamides is added.Mixed liquor is transferred to polytetrafluoroethylene (PTFE) lining
In stainless steel autoclave in, 100 DEG C react 3 hours.Reaction solution is cooled down, centrifugation adds excessive ethanol washing, product point
Dissipate and preserve in ethanol.
(2) a certain amount of Zn-In-S micron balls prepared are dispersed in the mixed liquor of 20mL first alcohol and waters, it is preferred that
Described ZIS amount is defined by that preferably can be dispersed in mixed liquor, and the volume ratio of wherein first alcohol and water is preferably 1:5, magnetic force
Stirring is lower add it is a certain amount of containing 0.2mmol silver nitrate solution, stir 10 minutes.Then mixed liquor is transferred to poly- four
In the stainless steel autoclave of PVF lining, 120 DEG C are reacted 3 hours.Product processing mode is ibid.
Product SEM figures are Fig. 1 upper lefts, and 50 minutes degradation rates are 99.3%.
Embodiment 2：
(1) indium nitrate of 2mmol zinc nitrate and 2mmol is dissolved in 40mL water, its pH is adjusted to 1 with hydrochloric acid；
Then add 10mL and contain 4mmol thioacetamides.Mixed liquor is transferred in the stainless steel autoclave of teflon lined,
100 DEG C are reacted 3 hours.Reaction solution is cooled down, centrifugation adds excessive ethanol washing, and product is scattered to be preserved in ethanol.
(2) a certain amount of Zn-In-S micron balls prepared are dispersed in the mixed liquor of 20mL first alcohol and waters, it is preferred that
Described ZIS amount is defined by that preferably can be dispersed in mixed liquor, and the volume ratio of wherein first alcohol and water is preferably 1:5, magnetic force
Stirring is lower add it is a certain amount of containing 1mmol silver nitrate solution, stir 10 minutes.Then mixed liquor is transferred to polytetrafluoro
In the stainless steel autoclave of vinyl liner, 150 DEG C are reacted 4 hours.Product processing mode is ibid.
Product SEM figures are Fig. 1 upper rights, and 50 minutes degradation rates are 99.1%.
Embodiment 3：
(1) inidum chloride of 2mmol zinc chloride and 1mmol is dissolved in 40mL water, its pH is adjusted to 2 with hydrochloric acid,
Then the solution that 10mL contains 2mmol thioacetamides and 4mmol thiocarbamides is added.Mixed liquor is transferred to teflon lined
In stainless steel autoclave, reacted 4 hours at 100 DEG C.Reaction solution is cooled down, centrifugation adds excessive ethanol washing, and product is dispersed in
Preserved in ethanol.
(2) a certain amount of Zn-In-S micron balls prepared are dispersed in the mixed liquor of 20mL first alcohol and waters, it is preferred that
Described ZIS amount is defined by that preferably can be dispersed in mixed liquor, and the volume ratio of wherein first alcohol and water is preferably 1:5, magnetic force
Stirring is lower add it is a certain amount of containing 5mmol silver nitrate solution, stir 10 minutes.Then mixed liquor is transferred to polytetrafluoro
In the stainless steel autoclave of vinyl liner, 120 DEG C are reacted 5 hours.Product processing mode is ibid.
Product SEM figures are Fig. 1 lower-lefts, and 50 minutes degradation rates are 99.9%.
Embodiment 4：
(1) indium acetate of 1mmol zinc acetate and 1mmol is dissolved in 40mL water, its pH is adjusted to 2 with hydrochloric acid,
Then the solution that 10mL contains 4mmol thioacetamides and 4mmol thiocarbamides is added.Mixed liquor is transferred to teflon lined
In stainless steel autoclave, reacted 6 hours at 100 DEG C.Reaction solution is cooled down, centrifugation adds excessive ethanol washing, and product is dispersed in
Preserved in ethanol.
(2) a certain amount of Zn-In-S micron balls prepared are dispersed in the mixed liquor of 20mL first alcohol and waters, it is preferred that
Described ZIS amount is defined by that preferably can be dispersed in mixed liquor, and the volume ratio of wherein first alcohol and water is preferably 1:5, magnetic force
Stirring is lower add it is a certain amount of containing 2mmol silver nitrate solution, stir 10 minutes.Then mixed liquor is transferred to polytetrafluoro
In the stainless steel autoclave of vinyl liner, 130 DEG C are reacted 7 hours.Product processing mode is ibid.
Product SEM figures are Fig. 1 bottom rights, and 50 minutes degradation rates are 99.5%.
Embodiment 5：
(1) indium nitrate of 1mmol zinc nitrate and 1mmol is dissolved in 40mL water, its pH is adjusted to 2 with hydrochloric acid,
Then the solution that 10mL contains 4mmol thioacetamides and 4mmol thiocarbamides is added.Mixed liquor is transferred to teflon lined
In stainless steel autoclave, reacted 4 hours at 80 DEG C.Reaction solution is cooled down, centrifugation adds excessive ethanol washing, and product is dispersed in
Preserved in ethanol.
(2) a certain amount of Zn-In-S micron balls prepared are dispersed in the mixed liquor of 20mL first alcohol and waters, it is preferred that
Described ZIS amount is defined by that preferably can be dispersed in mixed liquor, and the volume ratio of wherein first alcohol and water is preferably 1:5, magnetic force
Stirring is lower add it is a certain amount of containing 0.2mmol silver nitrate solution, stir 10 minutes.Then mixed liquor is transferred to poly- four
In the stainless steel autoclave of PVF lining, 180 DEG C are reacted 8 hours.Product processing mode is ibid.
Embodiment 6：
(1) indium nitrate of 1mmol zinc nitrate and 1mmol is dissolved in 40mL water, its pH is adjusted to 3 with hydrochloric acid,
Then the solution that 10mL contains 4mmol thioacetamides, 2mmol thiocarbamides and 2mmol vulcanized sodium is added.Mixed liquor is transferred to poly- four
In the stainless steel autoclave of PVF lining, reacted 4 hours at 80 DEG C.Reaction solution is cooled down, centrifugation adds excessive ethanol and washed
Wash, product is scattered to be preserved in ethanol.
(2) a certain amount of Zn-In-S micron balls prepared are dispersed in the mixed liquor of 20mL first alcohol and waters, it is preferred that
Described ZIS amount is defined by that preferably can be dispersed in mixed liquor, and the volume ratio of wherein first alcohol and water is preferably 1:5, magnetic force
Stirring is lower add it is a certain amount of containing 0.2mmol silver nitrate solution, stir 10 minutes.Then mixed liquor is transferred to poly- four
In the stainless steel autoclave of PVF lining, 150 DEG C are reacted 5 hours.Product processing mode is ibid.
Above-mentioned 6 embodiments are in order to show, by controlling reaction condition：The material of reaction temperature, time and reactant
Amount proportioning, the photochemical catalyst of different surface morphology and optical band gap can be obtained, so that applied to different light-catalyzed reactions.
Application examples 1
The photochemical catalyst of 20mg embodiment 1 is added in the aqueous solution of 50ppm rhodamine Bs, stirring a period of time, made
Dye molecule reaches adsorption equilibrium in photocatalyst surface, and control group is added without any photochemical catalyst, then under natural light or
Different time is irradiated under person's 500W tungsten halogen lamps, by the absorption spectra for measuring solution.As shown in figure 5, almost complete in 20 minutes
Degradable, degradation rate is 99.5%, and the dyestuff for being not added with catalyst only has 5% reduction, and this is due to molecular structure of dye quilt
Destroy to a certain extent, be commonly called as photobleaching.
All above-mentioned this intellectual properties of primarily implementation, the not this new product of implementation of setting limitation other forms
And/or new method.Those skilled in the art will utilize this important information, the above modification, to realize similar execution feelings
Condition.But, all modifications or transformation belong to the right of reservation based on new product of the present invention.
The above described is only a preferred embodiment of the present invention, being not the limitation for making other forms to the present invention, appoint
What those skilled in the art changed or be modified as possibly also with the technology contents of the disclosure above equivalent variations etc.
Imitate embodiment.But it is every without departing from technical solution of the present invention content, the technical spirit according to the present invention is to above example institute
Any simple modification, equivalent variations and the remodeling made, still fall within the protection domain of technical solution of the present invention.
Claims (7)
1. a kind of flower-shaped heterojunction structure micron ball photocatalyst of tree peony, it is characterised in that it is followed successively by Zn-In-S from inside to outside
The Ag-In-S outer layers of core, 20-200nm Zn-Ag-In-S intermediate layers and 10-50nm；Synthesize male by hydrothermal growth process first
Red flower-shaped Zn-In-S core micron balls, make its surface stack the class floweriness to be formed for thickness 50nm or so nanometer sheet self assembly
Valve layer structure, inside is solid；Then partial cation exchange process is utilized, by the Zn- of Zn-In-S core micron ball surface regions
In-S is transformed into Ag-In-S, and it is Zn-Ag-In-S intermediate layers to have a transition zone in the middle of this two layers.
2. the flower-shaped heterojunction structure micron ball photocatalyst of tree peony according to claim 1, it is characterised in that the micron ball
Size be 0.5-10 μm, pattern be that petal stratiform, specific surface area are 100-150m2/g。
3. a kind of preparation method of the flower-shaped heterojunction structure micron ball photocatalyst of any described tree peony of claim 1 or 2, specifically
Comprise the following steps：
(1) preparation of Zn-In-S micron balls：
By hydrothermal growth process, it is 1 to control reactant zinc salt, indium salts, the amount mol ratio of sulphur source:(0.8-3.2):(4-8)；Control
The pH value of reaction solution is between 0.5-3, reaction temperature is 100-180 DEG C, and the reaction time is 2-8 hours, obtains various sizes of
The flower-shaped Zn-In-S micron balls of tree peony；Alternately washing, the centrifugation of product ethanol and deionized water, is then stored in ethanol or goes
In ionized water；
(2) preparation of the heterogeneous microballoons of Zn-In-S/Ag-In-S：
Zn-In-S micron balls obtained by step (1) are dispersed in the mixed liquor of first alcohol and water, handed over by partial cation
Change, control adds 0.2-5mmol AgNO3And control solution acid alkalinity pH value between 0.5-3, reaction temperature be 100-180
DEG C, the reaction time is 2-8 hours, and control obtains the Ag-In-S layers of different-thickness；Product ethanol and deionized water are alternately washed
Wash, centrifuge, be then stored in ethanol or deionized water.
4. the preparation method of the flower-shaped heterojunction structure micron ball photocatalyst of tree peony as claimed in claim 3, it is characterised in that zinc
Salt is selected from one of zinc sulfate, zinc nitrate, zinc acetate or zinc chloride；Indium salts are selected from indium sulfate, indium nitrate, indium acetate or chlorination
One of indium, sulphur source is selected from one of thioacetamide, thiocarbamide or vulcanized sodium or composition；Indium salts and the mol ratio of zinc salt exist
Between 0.8-2.5, the amount of the material of sulphur source is 4-8 times of the amount of zinc salt material.
5. the preparation method of the flower-shaped heterojunction structure micron ball photocatalyst of tree peony as claimed in claim 3, it is characterised in that institute
The preparation for the heterogeneous microballoon of Zn-In-S micron balls and Zn-In-S/Ag-In-S stated is the stainless steel height in teflon lined
Press in kettle and synthesize.
6. the preparation method of the flower-shaped heterojunction structure micron ball photocatalyst of tree peony as claimed in claim 3, it is characterised in that sun
The reaction temperature of ion-exchange reactions is 120-160 DEG C, and the reaction time is 4-6 hours.
7. the flower-shaped heterojunction structure micron ball photocatalyst dyestuff in photocatalytic degradation contaminant water of tree peony described in claim 1
Using.
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| CN105950135B (en) * | 2016-05-09 | 2018-07-31 | 中国科学技术大学 | Quantum dot, the preparation method and use of nucleocapsid |
| CN109821553A (en) * | 2019-01-16 | 2019-05-31 | 上海理工大学 | A kind of ZnIn for thering is adsorption photochemical catalysis to act synergistically2S4The preparation method and its effect of microballoon |
| CN110735151A (en) * | 2019-06-20 | 2020-01-31 | 常州大学 | Preparation method of titanium carbide composite indium zinc sulfide photo-anode |
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