CN103055899A - Mesoporous nano spheroidal ZnxCd1-xS particle and preparation method and application thereof - Google Patents
Mesoporous nano spheroidal ZnxCd1-xS particle and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a mesoporous nano spheroidal ZnxCd1-xS particle and a preparation method and an application thereof. The ZnxCd1-xS particle is in a solid solution structure, X is equal to 0.0-1.0, the size of a crystal grain is in the range of 12.2-15.8nm, and the width of a forbidden band is in the range of 2.22-3.36eV. The mesoporous nano spheroidal ZnxCd1-xS particle can be applied to photocatalysis degradation reaction of organic waste water such as rhodamine, irgasan and the like under visible light. Compared with the prior art, the mesoporous nano spheroidal ZnxCd1-xS particle has the advantages and obvious effects that chemical reagents used in the invention are all regular reagents, low in cost, easy to obtain, simple in preparation technology, convenient to operate, stable in structure and easy to control.
Description
Technical field
The present invention relates to a kind of photochemical catalyst, be specially a kind of meso-porous nano ball-type Zn
xCd
1-xThe preparation method and application of S particle.The preparing technical field that belongs to semiconductor light-catalyst.
Background technology
Photocatalitic Technique of Semiconductor is multiple hazardous contaminant because powerful oxidability can be degraded, simultaneously, and its environmental friendliness, can utilize solar energy, characteristics such as reaction condition is gentle, and cost is low thereby have extremely wide application prospect are subject to the extensive concern of Chinese scholars day by day.Wherein, TiO
2Material is high because of photocatalytic activity, and stable in properties is nontoxic and material is cheap, becomes the current photochemical catalyst that has application potential most.But because TiO
2Energy gap own is larger, can only absorb ultraviolet light, and is low to the utilization rate of sunshine, thereby has larger limitation in actual applications.The non-TiO of Development of Novel
2The catalysis material of system is one of effective way that addresses this problem, to obtain higher practical value when significantly improving the visible light utilization rate.Chalcogenide such as CdS etc. are considered to excellent visible light catalyst, but have the problems such as photoetch is serious, poor stability.Studies show that, form the stability that polynary sulfide can obviously improve material by other metallic elements of bonding.The method of at present synthetic polynary sulfide adopts structure directing agent supplementary means low temperature synthetic more, thereby exists catalyst degree of crystallinity not high, and particle diameter is even not, the problems such as complex disposal process.The present invention utilizes the controlled phase behavior under the supercritical fluid HTHP, high diffusivity also can eliminate surface tension and prevent that effectively material structure from destroying, thereby forms the uniform nano particle of high-crystallinity.The present invention under the condition of non-structure directed agents, utilize the hot method one-step synthesis of supercritical solvent component adjustable, size is controlled, the continuously adjustable meso-porous nano ball-type of spectral absorption band edge Zn
xCd
1-xThe S photochemical catalyst has also significantly improved the stability of catalyst when improving the sunshine utilization rate, realized being repeatedly used.
Summary of the invention
The object of the invention is to for the existing defective of prior art and the market demand, provide that a kind of component is adjustable, size is controlled, continuous adjustable, the constitutionally stable meso-porous nano ball-type Zn of spectral absorption band edge
xCd
1-xS particle, another object of the present invention provide preparation method and the purposes of this particle.
Purpose of the present invention is achieved through the following technical solutions:
A kind of meso-porous nano ball-type Zn
xCd
1-xThe S particle is characterized in that: described Zn
xCd
1-xThe S particle is solid solution structure, X=0.0～1.0, and grain size range is 12.2～15.8nm, the energy gap scope is 2.22-3.36eV.
Above-mentioned meso-porous nano ball-type Zn
xCd
1-xThe preparation method of S particle comprises the steps:
1) be 1 * 10 with integral molar quantity
-3The Zn of mol (Ac)
22H
2O and Cd (Ac)
22H
2O is dissolved in the 30ml ethanol with different Zn/Cd mol ratios; 2) add 4 * 10
-3MolCH
3CSNH
2, stir under the room temperature to be placed in the autoclave that total measurement (volume) is 500mL in 10 minutes and react a period of time at a certain temperature; 3) naturally cool to room temperature, the sediment that obtains is centrifugal, respectively wash three times with ethanol and deionized water after in 80 ℃ of vacuum drying, can obtain meso-porous nano ball-type Zn
xCd
1-xThe S particle.
Above-mentioned Zn/Cd mol ratio is 0.0:1.0～1.0:0.0.
Above-mentioned reaction temperature is 230～260 ℃; Reaction time is 10～60 minutes.
The product of the present invention's preparation carries out structural characterization by following means: the X ray diffracting spectrum that adopts RigakuD/Max-RB type X-ray diffractometer to measure carries out the structural analysis of sample; Adopt the appearance structure of the electromicroscopic photograph analytic sample of JEM-2010 type transmission electron microscope acquisition; Adopt MC-2530 type UV-Vis DRS spectrometer (UV-vis DRS) to analyze absorbing properties.
Meso-porous nano ball-type Zn provided by the present invention
xCd
1-xThe S photochemical catalyst adopts following light-catalyzed reaction to investigate its catalytic performance.Take by weighing 50mg and 25mg Zn
xCd
1-xThe S catalyst adds respectively in 50mL 10mg/L simulative organic wastewater parachlorophenol solution and the rhodamine B solution and places the self-control quartz reactor.Under 30 ℃, at the uniform velocity stir 1h to adsorption equilibrium, open the 300W xenon lamp lasting light catalytic reaction 2h that is positioned at 18cm place directly over the reactor, and with the light of filter plate elimination wavelength less than 420nm.Timing sampling in the course of reaction is measured respectively the change in concentration of parachlorophenol and rhodamine B and is calculated degradation rate at 224nm and 553nm place with ultraviolet specrophotometer.Therefore the contaminant degradation that reaction only had less than 5% in 2 hours under unglazed photograph or catalyst-free condition can ignore the error that causes thus.In the life experiment with each reacted catalyst with after the washed with de-ionized water 3 times in 100 ℃ of oven dry 12h, continue afterwards to use.Each life experiment reaction time is 2h.
This shows described meso-porous nano ball-type Zn
xCd
1-xThe S particle can be applicable under the visible light photocatalytic degradation reaction to organic wastewaters such as rhodamine B, parachlorophenols.
The present invention compared with prior art, have the following advantages and outstanding effect: chemical reagent used in the present invention is common agents, cheap and easy to get, preparation technology is simple, easy to operate, Stability Analysis of Structures is easily controlled.
Description of drawings
Fig. 1 is the XRD collection of illustrative plates of the prepared sample of embodiment 1-6;
Fig. 2 is (a) transmission electron microscope of embodiment 1 prepared sample and (b) high power transmission electron microscope photo;
Fig. 3 is the UV-vis DRS collection of illustrative plates of the prepared sample of embodiment 1-6;
Fig. 4 is that the photocatalytic activity of the prepared sample rhodamine B degradation of embodiment 1-6 compares;
Fig. 5 is that the photocatalytic activity of the prepared sample degraded of embodiment 1-6 parachlorophenol compares;
Fig. 6 is that the photocatalytic activity of embodiment 1 and the prepared sample rhodamine B degradation of embodiment 7-8 compares;
Fig. 7 is that the photocatalytic activity of embodiment 1 and the obtained sample rhodamine B degradation of embodiment 9-10 compares;
Fig. 8 is the performance in service life of embodiment 1 prepared sample rhodamine B degradation.
The specific embodiment:
Below in conjunction with specific embodiment the present invention is done further in detail, illustrates clearly and completely, listed embodiment only is further described the present invention, and is not thereby limiting the invention:
Be 1 * 10 with integral molar quantity
-3The Zn of mol (Ac)
22H
2O and Cd (Ac)
22H
2O is dissolved in the 30ml ethanol, and the Zn/Cd mol ratio is 0.21:0.79.Add afterwards 4 * 10
-3MolCH
3CSNH
2, stir under the room temperature to be placed in 10 minutes in the autoclave that total measurement (volume) is 500mL and under 245 ℃, reacted 10 minutes.Naturally cool to subsequently room temperature, the sediment that obtains is centrifugal, respectively wash three times with ethanol and deionized water after in 80 ℃ of vacuum drying, can obtain object-meso-porous nano ball-type Zn
0.21Cd
0.79The S photochemical catalyst.The X-ray diffracting spectrum of the prepared sample of the present embodiment shows that the gained sample is the homogeneous phase solid solution structure of high-crystallinity among Fig. 1, crystal grain diameter 15.2nm.Fig. 2 is the TEM photo of the prepared sample of the present embodiment, is the nanometer ball shape structure with mesopore orbit that uniform nano particle consists of from the visible gained sample of photo, and sphere diameter is 300～400nm.The HRTEM photo shows that the interplanar distance of sample is 0.33nm.Can find out that by UV-vis DRS collection of illustrative plates among Fig. 3 the prepared sample of the present embodiment has very strong visible absorption performance, energy gap is 2.35eV.Fig. 4 and Fig. 5 show that respectively the present embodiment has better photocatalytic activity than embodiment 2-6 in the reaction of rhodamine B degradation and parachlorophenol.Fig. 6 shows that the present embodiment has better photocatalytic activity than embodiment 7-8 in the reaction of rhodamine B degradation.Fig. 7 shows that the present embodiment has better photocatalytic activity than embodiment 9-10 in the reaction of rhodamine B degradation.Fig. 8 is the life test result of the present embodiment rhodamine B degradation, can find out that the prepared photochemical catalyst of the present embodiment has stable photocatalytic activity.
The Zn/Cd mol ratio changed into be 0.0:1.0, be i.e. pure CdS catalyst.All the other contents are described identical with embodiment 1.X-ray diffracting spectrum shows that the resulting CdS of the present embodiment is six side's phase CdS crystal (PDF No.41-1049) of high-crystallinity among Fig. 1, crystal grain diameter 15.8nm.UV-vis DRS collection of illustrative plates shows that the prepared sample of the present embodiment has very strong visible absorption performance among Fig. 3, and energy gap is 2.22eV.
The Zn/Cd mol ratio changed into be 0.11:0.89, all the other contents are described identical with embodiment 1.The X-ray diffracting spectrum of the prepared sample of the present embodiment shows that the gained sample is the homogeneous phase solid solution structure of high-crystallinity among Fig. 1, crystal grain diameter 15.3nm.UV-vis DRS collection of illustrative plates shows that the prepared sample of the present embodiment has very strong visible absorption performance among Fig. 3, and energy gap is 2.31eV.
The Zn/Cd mol ratio changed into be 0.29:0.71, all the other contents are described identical with embodiment 1.The X-ray diffracting spectrum of the prepared sample of the present embodiment shows that the gained sample is the homogeneous phase solid solution structure of high-crystallinity among Fig. 1, crystal grain diameter 14.7nm.UV-vis DRS collection of illustrative plates shows that the prepared sample of the present embodiment has very strong visible absorption performance among Fig. 3, and energy gap is 2.41eV.
The Zn/Cd mol ratio changed into be 0.41:0.59, all the other contents are described identical with embodiment 1.The X-ray diffracting spectrum of the prepared sample of the present embodiment shows that the gained sample is the homogeneous phase solid solution structure of high-crystallinity among Fig. 1, crystal grain diameter 13.8nm.UV-vis DRS collection of illustrative plates shows that the prepared sample of the present embodiment has very strong visible absorption performance among Fig. 3, and energy gap is 2.49eV.
The Zn/Cd mol ratio changed into be 1.0:0.0, be i.e. pure ZnS catalyst.All the other contents are described identical with embodiment 1.X-ray diffracting spectrum shows that the prepared ZnS sample of the present embodiment is the Emission in Cubic ZnS crystal (PDF No.65-0309) of high-crystallinity among Fig. 1, crystal grain diameter 12.2nm.The prepared sample of the present embodiment is without the visible absorption performance in the UV-vis DRS collection of illustrative plates among Fig. 3, and energy gap is 3.36eV.
Embodiment 7
Change reaction temperature into 230 ℃, all the other contents are described identical with embodiment 1.
Embodiment 8
Change reaction temperature into 260 ℃, all the other contents are described identical with embodiment 1.
Embodiment 9
To change 30 minutes the reaction time into, all the other contents are described identical with embodiment 1.
Embodiment 10
To change 60 minutes the reaction time into, all the other contents are described identical with embodiment 1.
Embodiment 11
Take by weighing resulting meso-porous nano ball-type Zn among 50mg and the 25mg above-described embodiment 1-10
xCd
1-xThe S photochemical catalyst adds respectively 50mL 10mg/L simulative organic wastewater parachlorophenol solution and rhodamine B solution.To adsorption equilibrium, start light-catalyzed reaction at the uniform velocity stirring 1h under 30 ℃, adopt a 300W xenon lamp as light source, and with the light of filter plate elimination wavelength less than 420nm.Reaction time is 2h.Timing sampling in the course of reaction is measured respectively the change in concentration of parachlorophenol and rhodamine B and is calculated degradation rate at 224nm and 553nm place with ultraviolet specrophotometer.The photocatalytic degradation result that the prepared sample of embodiment 1-6 is used for rhodamine B (Fig. 4) and parachlorophenol (Fig. 5) shows, the pure ZnS of embodiment 6() without obvious visible light activity, embodiment 1-5 all has good visible light catalysis activity, wherein the prepared Zn of embodiment 1
0.21Cd
0.79S has best photocatalytic activity.Fig. 6 be the sample rhodamine B degradation that obtains of differential responses temperature specific activity, can find out that embodiment 1 has better photocatalysis performance than the embodiment 7-8 of other temperature preparation.Fig. 7 be the sample rhodamine B degradation that obtains the differential responses time specific activity, can find out that embodiment 1 has better photocatalysis performance than other embodiment 9-10.
Embodiment 12
Adopt embodiment 1 prepared sample to carry out life experiment, will each reacted catalyst in the life experiment with after the washed with de-ionized water 3 times in 100 ℃ of oven dry 12h, continue afterwards use.Each life experiment reaction time is 2h, and the experiment cycle-index is 6 times, the results are shown in Figure 8.Can find out that the resulting catalyst of the present invention has stable visible light catalysis activity.
Claims (5)
1. meso-porous nano ball-type Zn
xCd
1-xThe S particle is characterized in that: described Zn
xCd
1-xThe S particle is solid solution structure, X=0.0～1.0, and grain size range is 12.2～15.8nm, the energy gap scope is 2.22～3.36eV.
2. one kind prepares the described meso-porous nano ball-type of claim 1 Zn
xCd
1-xThe method of S particle is characterized in that: its step is as follows:
1) be 1 * 10 with integral molar quantity
-3The Zn of mol (Ac)
22H
2O and Cd (Ac)
22H
2O is dissolved in the 30ml ethanol with different Zn/Cd mol ratios; 2) add 4 * 10
-3MolCH
3CSNH
2, stir under the room temperature to be placed in the autoclave that total measurement (volume) is 500mL in 10 minutes and react a period of time at a certain temperature; 3) naturally cool to room temperature, the sediment that obtains is centrifugal, respectively wash three times with ethanol and deionized water after in 80 ℃ of vacuum drying, can obtain meso-porous nano ball-type Zn
xCd
1-xThe S particle.
3. meso-porous nano ball-type Zn according to claim 2
xCd
1-xThe preparation method of S particle is characterized in that: in the step 1), described Zn/Cd mol ratio is 0.0:1.0～1.0:0.0.
4. meso-porous nano ball-type Zn according to claim 2
xCd
1-xThe preparation method of S particle is characterized in that: step 2) in, described reaction temperature is 230～260 ℃; Reaction time is 10～60 minutes.
5. meso-porous nano ball-type Zn according to claim 1
xCd
1-xThe meso-porous nano ball-type Zn that preparation method that one of S particle or claim 2-4 are any obtains
xCd
1-xThe S particle is characterized in that: described meso-porous nano ball-type Zn
xCd
1-xThe S particle is applied under the visible light photocatalytic degradation reaction to organic wastewaters such as rhodamine B, parachlorophenols.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103316694A (en) * | 2013-07-11 | 2013-09-25 | 吉林大学 | Preparation method of composite material of Zn0.8Cd0.2S and graphene |
| CN103433061A (en) * | 2013-09-18 | 2013-12-11 | 哈尔滨工业大学 | CdxZn1-xS:La solid solution photocatalyst and preparation method thereof |
| CN104888810A (en) * | 2015-05-06 | 2015-09-09 | 赵伟杰 | Fe-doped zinc-based sulfide photocatalyst, preparation method and application thereof |
| CN105879883A (en) * | 2016-04-06 | 2016-08-24 | 扬州大学 | Novel visible light degradation methylene blue photocatalyst alpha-EuZrS3 |
| CN109529890A (en) * | 2018-11-06 | 2019-03-29 | 常州大学 | A kind of preparation method of zinc-cadmium sulfide/bismuth oxybromide composite visible light catalyst |
| CN109622015A (en) * | 2018-12-14 | 2019-04-16 | 哈尔滨理工大学 | A kind of preparation method of cadmium doped zinc sulphide/carbonitride |
| CN110102316A (en) * | 2019-05-07 | 2019-08-09 | 东莞理工学院 | A kind of preparation method of the spherical zinc-cadmium sulfide solid solution of porous nano |
| CN113368873A (en) * | 2021-07-02 | 2021-09-10 | 安徽理工大学环境友好材料与职业健康研究院(芜湖) | Visible light assisted Fenton cocatalyst and preparation method and application thereof |
| CN113617365A (en) * | 2021-08-24 | 2021-11-09 | 青岛科技大学 | Porous Cd with stacking faults1-xZnxS/GO composite material and preparation method thereof |
| CN114100643A (en) * | 2021-09-26 | 2022-03-01 | 东莞理工学院 | Preparation method of catalyst for photocatalytic decomposition of pure water |
| CN115888759A (en) * | 2022-11-15 | 2023-04-04 | 南昌大学 | Synthesis method of alternately bridged cadmium sulfide-zinc oxide heterojunction periodic macroporous photocatalytic hydrogen evolution material |
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Cited By (15)
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| CN103316694A (en) * | 2013-07-11 | 2013-09-25 | 吉林大学 | Preparation method of composite material of Zn0.8Cd0.2S and graphene |
| CN103433061A (en) * | 2013-09-18 | 2013-12-11 | 哈尔滨工业大学 | CdxZn1-xS:La solid solution photocatalyst and preparation method thereof |
| CN103433061B (en) * | 2013-09-18 | 2015-05-27 | 哈尔滨工业大学 | CdxZn1-xS:La solid solution photocatalyst and preparation method thereof |
| CN104888810A (en) * | 2015-05-06 | 2015-09-09 | 赵伟杰 | Fe-doped zinc-based sulfide photocatalyst, preparation method and application thereof |
| CN105879883A (en) * | 2016-04-06 | 2016-08-24 | 扬州大学 | Novel visible light degradation methylene blue photocatalyst alpha-EuZrS3 |
| CN105879883B (en) * | 2016-04-06 | 2018-07-20 | 扬州大学 | A kind of Visible Light Induced Photocatalytic methylene blue photochemical catalyst α-EuZrS3 |
| CN109529890A (en) * | 2018-11-06 | 2019-03-29 | 常州大学 | A kind of preparation method of zinc-cadmium sulfide/bismuth oxybromide composite visible light catalyst |
| CN109622015A (en) * | 2018-12-14 | 2019-04-16 | 哈尔滨理工大学 | A kind of preparation method of cadmium doped zinc sulphide/carbonitride |
| CN110102316A (en) * | 2019-05-07 | 2019-08-09 | 东莞理工学院 | A kind of preparation method of the spherical zinc-cadmium sulfide solid solution of porous nano |
| CN113368873A (en) * | 2021-07-02 | 2021-09-10 | 安徽理工大学环境友好材料与职业健康研究院(芜湖) | Visible light assisted Fenton cocatalyst and preparation method and application thereof |
| CN113617365A (en) * | 2021-08-24 | 2021-11-09 | 青岛科技大学 | Porous Cd with stacking faults1-xZnxS/GO composite material and preparation method thereof |
| CN113617365B (en) * | 2021-08-24 | 2023-08-04 | 青岛科技大学 | Porous Cd with stacking fault 1-x Zn x S/GO composite material and preparation method thereof |
| CN114100643A (en) * | 2021-09-26 | 2022-03-01 | 东莞理工学院 | Preparation method of catalyst for photocatalytic decomposition of pure water |
| CN114100643B (en) * | 2021-09-26 | 2023-06-02 | 东莞理工学院 | Preparation method of catalyst for photocatalytic decomposition of pure water |
| CN115888759A (en) * | 2022-11-15 | 2023-04-04 | 南昌大学 | Synthesis method of alternately bridged cadmium sulfide-zinc oxide heterojunction periodic macroporous photocatalytic hydrogen evolution material |
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Application publication date: 20130424 |