CN106391118B - Class zeolite cadmium chalcogenide, preparation method and application - Google Patents
Class zeolite cadmium chalcogenide, preparation method and application Download PDFInfo
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Abstract
The invention discloses a kind of novel class zeolite cadmium chalcogenide, the molecular formula of the compound is [Cd8S(SPh)14]Cd(2Me‑Im)4, wherein 2Me-Im is 2-methylimidazole, and skeleton structure is by super tetrahedron [Cd8S(SPh)14]2+Cluster and Cd2+It is constructed by 2-methylimidazole anion bridging, is a kind of 4 novel connection class zeolite topologicals.It is found through experiment that there is efficient photocatalysis property under class zeolite cadmium chalcogenide room temperature of the present invention, it can degradable organic pollutant methyl orange.
Description
Technical field
The invention belongs to inorganic microporous field of material technology, and in particular to a type zeolite cadmium chalcogenide materials, its system
Preparation Method and application.
Background technique
Micropore chalcogenide is a kind of important inorganic functional material, and not only structure is very rich, but also has and partly lead
Volume property, and prospect is had important application in fields such as selective ion exchange, fast ion conduction and visible light catalytics
[A.K.Cheetham,G.Férey,T.Loiseau,Angew.Chem.,Int.Ed.,1999,38,3268-3292；P.Feng,
X.Bu,N.Zheng,Acc.Chem.Res.,2005,38,293-303；Q.Lin,X.Bu,C.Mao,X.Zhao,K.Sasan,
P.Feng,J.Am.Chem.Soc.2015,137,6184-6187；F.Wang,J.Lin,T.Zhao,D.Hu,T.Wu,Y.Liu,
J.Am.Chem.Soc.,2016,138,7718–7724.].Wherein cadmium chalcogenide is due to being weight with photoelectric effect outstanding
The quantum dot and photoelectrocatalysimaterial material wanted have important in practical applications and are widely worth.[M.Moriya,
T.Minegishi,H.Kumagai,M.Katayama,J.Kubota,K.Domen,J.Am.Chem.Soc.,2013,135,
3733–3735；K.Wu,Z.Chen,H.Lv,H.Zhu,C.L Hill,T.Lian,J.Am.Chem.Soc.,2014,136,
7708–7716；F.Jiang,G.T.Harada,Y.Kuang,T.Minegishi,K.Domen,S.Ikeda
J.Am.Chem.Soc.,2015,137,13691–13697；F.Qiu,Z.Han,J.J.Peterson,M.Y.Odoi,
K.L.Sowers,T.D.Krauss,Nano Lett.,2016,16,5347–5352].Class zeolite type cadmium chalcogenide is not only simultaneous
The semiconductor property of standby chalcogenide, and can be combined with its unique cellular structure, by inhibiting the compound of light induced electron
Effectively improve its photoelectric conversion efficiency, thus make its photoelectrocatalysis property significantly improve [Q.Zhang, Z.Lin, X.Bu,
T.Wu,P.Feng,Chem.Mater.,2008,20,3239–3241；Q.Zhang,X.Bu,J.Zhang,T.Wu,P.Feng,
J.Am.Chem.Soc.,2007,129,8412–8413；N.Zheng,H.Lu,X.Bu,P.Feng,J.Am.Chem.Soc.,
2006,128,4528–4529；T.Wu,R.Khazhakyan,L.Wang,X.Bu,S.-T.Zheng,V.Chau,P.Feng,
Angew.Chem.Int.Ed.2011,50,2536–2539].The synthesis and property of class zeolite cadmium chalcogenide material are studied, it will
New approach is provided for the further research and development of novel optoelectronic materials, such as: photoelectrocatalysis (optoelectronic catalysis),
Optoelectronic switch (optoelectronic switch), photic electroluminescent material (PL, EL), chemical sensor
(Chemsensor), [Zheng, the N.F. such as；Bu,X.H.；Feng,P.Y.Nature,2003,426,428-431；N.Zheng,
X.Bu,H.Vu,P.Feng,Angew.Chem.Int.Ed.,2005,44,5299–5303J.F.Corrigan,O.Fuhr,
D.Fenske,Adv.Mater.,2009,21,1867–1871].It designs and closes in conjunction with the characteristic of bridging ligand and Tetrahedral atoms cluster
At class zeolite cadmium chalcogenide materials new thinking will be provided to develop novel and multifunctional material.
Summary of the invention
It is an object of that present invention to provide a type zeolite cadmium chalcogenide materials, preparation method and application, the chemical combination
Object has the class zeolite topological of novel 4- connection, has stable and efficient photocatalysis property under room temperature, can have
The drop photocatalysis solution organic pollutant methyl orange of effect.
To achieve the above object, the present invention adopts the following technical scheme:
One type zeolite cadmium chalcogenide, molecular formula are [Cd8S(SPh)14]Cd(2Me-Im)4, wherein 2Me-Im is 2-
Methylimidazole, skeleton structure is by super tetrahedron [Cd8S(SPh)14]2+Cluster and Cd2+Pass through 2-methylimidazole anion bridge
Company constructs, and is a kind of class zeolite topological of novel 4- connection.Further, the novel class zeolite cadmium chalcogenide
Crystal category cubic system, space group Pa-3, cell parameter are as follows:α=90.0 °.
The preparation method of above-mentioned class zeolite cadmium chalcogenide specifically comprises the following steps: Cd (SPh)2、Na2S2O3、2-
Methylimidazole, triethylamine and acetonitrile solution are uniformly mixed, then in 85-100 DEG C isothermal reaction 120-180 hour, react
After product is washed, is drying to obtain.
Specifically, the Cd (SPh)2、Na2S2O3Molar ratio with 2-methylimidazole is 5-7:1:8-12, preferably 6:1:
10。
Specifically, acetonitrile solution and triethylamine are used as solvent, every 0.01mmol Na2S2O3Add 0.8-1.5mL acetonitrile
Aqueous solution, 0.3-0.5mL triethylamine；The acetonitrile solution is that 3:1 is mixed by volume by acetonitrile and water.
Above-mentioned class zeolite cadmium chalcogenide answering in terms of degradable organic pollutant methyl orange as photocatalyst material
With.
Compared to the prior art, beneficial effects of the present invention are as follows:
The present invention is synthesized using low-temperature solvent thermal method, and reaction temperature is only 85-100 DEG C, and this method is different from document report
In the methods of common high temperature hydro-thermal, overcome the disadvantages of temperature is high, risk is big, low yield, repeatability difference.System of the present invention
Preparation Method simple process, mild condition, yield is higher, favorable repeatability, and class zeolite cadmium chalcogenide has at room temperature
Stable photocatalysis performance, can effectively degradable organic pollutant methyl orange, can be used as catalysis material use, be material science
New vitality is injected in the development in field.
Detailed description of the invention
Fig. 1 be the class zeolite cadmium chalcogenide skeleton structure diagram (display structure for clarity avoids covering, part
The C atom of hydrogen atom and thiophenol ligand is omitted)；
Fig. 2 is the topological structure of the skeleton of the class zeolite cadmium chalcogenide；
Fig. 3 is the XRD diagram of the class zeolite cadmium chalcogenide；
Fig. 4 is the class zeolite cadmium chalcogenide ultraviolet-visible spectrogram；
Fig. 5 is light degradation effect picture of the class zeolite cadmium chalcogenide to methyl orange.
Specific embodiment
In order to keep technical purpose of the invention, technical scheme and beneficial effects clearer, with reference to the accompanying drawing and specifically
Embodiment is further illustrated technical solution of the present invention, but the embodiment is intended to explain the present invention, and cannot manage
Solution is limitation of the present invention, in the examples where no specific technique or condition is specified, described according to the literature in the art
Technology or conditions carry out, reagents or instruments used without specified manufacturer according to product description, are that can pass through
The conventional products of commercially available acquisition.
Embodiment 1
The preparation method of one type zeolite cadmium chalcogenide, specifically:
0.06mmol Cd (SPh) is added first into horminess glass tube2(according to document Inorg.Chem.1987,26,
Method in 4057-4064. is synthesized), 0.01mmol Na2S2O3(Jinan Heng Hua Science and Technology Ltd.), 0.1mmol 2-
Methylimidazole (Sinopharm Chemical Reagent Co., Ltd.), 0.5mL triethylamine (Tianjin Fu Yu Fine Chemical Co., Ltd) and
1.0mL acetonitrile solution (volume ratio of acetonitrile and water is 3:1, and acetonitrile is purchased from Tianjin Fu Yu Fine Chemical Co., Ltd), glass
The filling rate of glass pipe is 10%.Ultrasonic disperse is uniform, and then tube sealing (seals glass tube, reacts to make on alcolhol burner
It is carried out under air-tight state).It being put into reaction kettle, constant temperature is placed 150 hours in 100 DEG C of drying boxes (being not necessarily to vacuum),
After naturally cool to room temperature, observing in glass tube has colourless cubic block shape crystal, with ethanol washing, is drying to obtain.
The yield of gained class zeolite cadmium chalcogenide is 69%, molecular formula are as follows: [Cd8S(SPh)14]Cd(2Me-Im)4.It sweeps
Retouching Electronic Speculum photoelectron spectroscopy (EDS), Cd:S is 3:5 in compound as the result is shown；Elemental analysis is as the result is shown in compound, and: C is
41.5%, H 3.0%, N 3.8% is consistent with the result of structural analysis.
The structure determination of gained class zeolite cadmium chalcogenide:
The class zeolite cadmium chalcogenide single crystal for choosing suitable size under the microscope, at room temperature in Bruker APEX II
The face CCD is visited on diffractometer, with the Mo-K alpha ray through graphite monochromator monochromatizationIt is collected and is spread out in a manner of ω
Penetrate data.All diffraction datas carry out semiempirical absorption correction using SADABS program.Cell parameter is determined with least square method.
Data convert and structure elucidation use SAINT and SHELXTL program to complete respectively.Crystal structure is solved with direct method, and metal is former
The position of son is determined by the E-map of direct method, and other non-hydrogen atoms then utilize difference Fourier function method and least square
Method determines, then carries out anisotropy refine, finally determines hydrogen atom position with theoretical hydrogenation method.Detailed gained compound
Axonometry data are shown in Table 1, and XRD diagram is as shown in figure 3, the characteristic peak of laboratory sample spectrogram and the characteristic peak of analogue spectrums are mutually right
It answers, illustrates that the crystal of compound is pure phase.Structure chart such as Fig. 1, gained compound are by super tetrahedron [Cd8S(SPh)14]2+Atom
Cluster and Cd2+It is constructed by 2-methylimidazole anion bridging.Super tetrahedron [Cd8S(SPh)14]2+Cluster is typical
The cluster of P1 configuration, by SCd4Tetrahedral each face is by a Cd (SPh)4Tetrahedron nut cap is formed, the difference is that super four sides
Four vertex positions of body are by 2Me-Im-Replace, super tetrahedron [Cd in structure8S(SPh)14]2+Pass through the 2Me-Im of Bridge 2 even-With
Tetrahedral Cd2+Connection, if by super tetrahedron [Cd8S(SPh)14]2+With discrete Cd2+Ion is respectively all as 4- connection
Node, 2Me-Im-Ligand regards line as, then the skeleton structure can simplify into a kind of novel class zeolite topological, such as Fig. 2 institute
Show.
1 compound [Cd of table8S(SPh)14]Cd(2Me-Im)4Crystallographic data
As shown in Table 1, the molecular formula of the class zeolite cadmium chalcogenide is C100H90N8Cd9S15, its crystal category cubic crystal
System, space group Pa-3, cell parameter are as follows:α=90.0 °；The bone of the class zeolite cadmium chalcogenide
Frame is a kind of zeolite type topology of novel 4- connection.
The uv-vis spectra of gained class zeolite cadmium chalcogenide measures:
After the dry ground processing of class zeolite cadmium chalcogenide sample, uv-vis spectra measurement is carried out, outside solid violet
Visible spectrum spectrogram is as shown in figure 4, compound has strong absorption, ABSORPTION EDGE 380nm in ultra-violet (UV) band.
Embodiment 2
The preparation method of one type zeolite cadmium chalcogenide, specifically:
0.06mmol Cd (SPh) is added first into horminess glass tube2(according to document Inorg.Chem.1987,26,
In 4057-4064. method synthesis), 0.01mmol Na2S2O3, 0.1mmol 2-methylimidazole, 0.5mL triethylamine and 1.0mL
Acetonitrile water mixed solution (volume ratio 3:1), the filling rate of glass tube are 10%, and ultrasonic disperse is uniform.Then on alcolhol burner
Tube sealing.It is put into reaction kettle, constant temperature is placed 120 hours in 85 DEG C of (being not necessarily to vacuum), after naturally cool to room temperature, observation
To there is colourless cubic block shape crystal, with ethanol washing, it is drying to obtain.Gained compound yield is 56%.
Embodiment 3
The preparation method of one type zeolite cadmium chalcogenide, specifically:
0.05mmol Cd (SPh) is added first into horminess glass tube2(according to document Inorg.Chem.1987,26,
In 4057-4064. method synthesis), 0.01mmol Na2S2O3, 0.08mmol 2-methylimidazole, 0.3mL triethylamine and
1.5mL acetonitrile water mixed solution (volume ratio 3:1), the filling rate of glass tube are 10%, and ultrasonic disperse is uniform.Then in alcohol
Tube sealing on lamp.It being put into reaction kettle, constant temperature is placed 180 hours in 85 DEG C of (be not necessarily to vacuum), after naturally cool to room temperature,
It has observed colourless cubic block shape crystal, with ethanol washing, has been drying to obtain.Gained compound yield is 58.2%.
Embodiment 4
The preparation method of one type zeolite cadmium chalcogenide, specifically:
0.07mmol Cd (SPh) is added first into horminess glass tube2(according to document Inorg.Chem.1987,26,
In 4057-4064. method synthesis), 0.01mmol Na2S2O3, 0.12mmol 2-methylimidazole, 0.4mL triethylamine and
0.8mL acetonitrile water mixed solution (volume ratio 3:1), the filling rate of glass tube are 10%, and ultrasonic disperse is uniform.Then in alcohol
Tube sealing on lamp.It being put into reaction kettle, constant temperature is placed 160 hours in 90 DEG C of (be not necessarily to vacuum), after naturally cool to room temperature,
It has observed colourless cubic block shape crystal, with ethanol washing, has been drying to obtain.Gained compound yield is 57%.
Application test
1 gained class zeolite cadmium chalcogenide (i.e. following samples) of the embodiment of the present invention is organic as catalysis material progress
The light degradation of pollutant methyl orange is tested.
Test method
Compound carries out the light degradation experiment of organic pollutant methyl orange at room temperature: configuration methyl orange solution
18.6735mg L-1, the sample for weighing 0.1g class zeolite cadmium chalcogenide is placed in 25mL methyl orange solution, ultrasonication with
It is uniformly mixed, obtains suspension.Use 400W Xe lamp as light source, in degradation experiment, sample solution persistently use magnetic stirrer into
Row stirring, took primary first-order equation liquid every 15 minutes, with ultraviolet-visible spectrum analysis (Shimadzu 2550) to the concentration of methyl orange
Carry out quantitative analysis.Experimental result is as shown in Figure 5.
As can be seen from Figure 5: compound has significant photocatalysis property to methyl orange, at room temperature to methyl orange
There is higher degradation efficiency, reach within 15 minutes 50% or more, reaches 90% within 45 minutes.In addition, preparing gained to embodiment 2 to 4
Class zeolite cadmium chalcogenide equally tested, the results showed that its degradation effect is suitable with the degradation efficiency of embodiment 1.This
It is the presence because of microcellular structure, restrained effectively the compound of light induced electron, improve semiconductor chalcogenide significantly
Photocatalysis property.Therefore, class zeolite chalcogenide of the present invention has photocatalysis property, can effectively degradable organic pollutant methyl
Orange can be used as photochemical catalyst use.
It should be noted last that: technical solution of the present invention that the above embodiments are only illustrative and not limiting is any right
The equivalent replacement and do not depart from the modification of spirit and scope of the invention or locally replace that the present invention carries out, should all cover in this hair
Within bright protective scope of the claims.
Claims (5)
1. a type zeolite cadmium chalcogenide, which is characterized in that molecular formula is [Cd8S(SPh)14]Cd(2Me-Im)4, wherein 2Me-
Im is 2-methylimidazole, and the skeleton structure of the class zeolite cadmium chalcogenide is by super tetrahedron [Cd8S(SPh)14]2+Cluster and
Cd2+It is constructed by 2-methylimidazole anion bridging.
2. the preparation method of class zeolite cadmium chalcogenide described in claim 1, which is characterized in that by Cd (SPh)2、Na2S2O3、2-
Methylimidazole, triethylamine and acetonitrile solution are uniformly mixed, then in 85-100 DEG C isothermal reaction 120-180 hour, react
After product is washed, is drying to obtain.
3. the preparation method of class zeolite cadmium chalcogenide according to claim 2, which is characterized in that the Cd (SPh)2、
Na2S2O3Molar ratio with 2-methylimidazole is 5-7:1:8-12.
4. the preparation method of class zeolite cadmium chalcogenide according to claim 2, which is characterized in that every 0.01 mmol
Na2S2O3Add 0.8-1.5 mL acetonitrile solution, 0.3-0.5 mL triethylamine；The acetonitrile solution is by acetonitrile and water
3:1 is mixed by volume.
5. class zeolite cadmium chalcogenide described in claim 1 is as photocatalyst material in degradable organic pollutant methyl orange side
The application in face.
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Citations (2)
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| WO2009120716A1 (en) * | 2008-03-24 | 2009-10-01 | Rutgers, The State University Of New Jersey | Compositions and methods for generating white light |
| CN105367591A (en) * | 2015-12-08 | 2016-03-02 | 安阳师范学院 | Cadimium complex monocrystal capable of catalyzing photodegradation of methylene blue, and preparation method thereof |
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| KR20070042333A (en) * | 2005-10-18 | 2007-04-23 | 삼성코닝 주식회사 | Chalcogenide precursor compound and preparation method of chalcogenide thin film using the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009120716A1 (en) * | 2008-03-24 | 2009-10-01 | Rutgers, The State University Of New Jersey | Compositions and methods for generating white light |
| CN105367591A (en) * | 2015-12-08 | 2016-03-02 | 安阳师范学院 | Cadimium complex monocrystal capable of catalyzing photodegradation of methylene blue, and preparation method thereof |
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| Title |
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| Hybrid materials through linkage of chalcogenide tetrahedral clusters;Paz Vaqueiro;《Dalton Transactions》;20100415;第39卷(第26期);5965-5972 * |
| One-Dimensional Assembly of Chalcogenide Nanoclusters with Bifunctional;Pingyun Feng et al.;《J. AM. CHEM. SOC》;20051007;第127卷(第43期);14990-14991 * |
| Three-Dimensional Covalent Co-Assembly between Inorganic Supertetrahedral Clusters and Imidazolates;Pingyun Feng et al.;《Angew. Chem. Int. Ed.》;20110223;第50卷;2536-2539 * |
| Two-dimensional assembly of tetrahedral chalcogenide clusters with tetrakis (imidazolyl)borate ligands;Zhien Lin et al.;《Dalton Trans.》;20111212;第41卷;3942-3944 * |
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