CN105289752B - A kind of organic-inorganic hybrid material with photocatalytic activity and its preparation method and application in the sunlight - Google Patents
A kind of organic-inorganic hybrid material with photocatalytic activity and its preparation method and application in the sunlight Download PDFInfo
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- CN105289752B CN105289752B CN201510588254.4A CN201510588254A CN105289752B CN 105289752 B CN105289752 B CN 105289752B CN 201510588254 A CN201510588254 A CN 201510588254A CN 105289752 B CN105289752 B CN 105289752B
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Abstract
The invention discloses a kind of organic-inorganic hybrid material with photocatalytic activity and its preparation method and application in the sunlight, its molecular formula is C42H54Cu8I14N6, construction unit is, near saturated solution is obtained by dissolving both cation, DMF solution dissolved metal salt, regulation ratios with methanol solution, clarified solution is filtered to obtain with filter paper, stand the organic-inorganic hybrid material that solvent flashing obtains target product cuprous iodide.Preparation method of the invention is simple and easy to apply, and obtained organic-inorganic hybrid material stability preferably, is not decomposed substantially below 200 DEG C, keeps stabilization, and good activity is shown in the organic wastewater that photocatalytic degradation contains methyl orange.
Description
Technical field
The invention belongs to catalysis material technical field, and in particular to a kind of organic with photocatalytic activity in the sunlight
Inorganic hybrid material and its preparation method and application.
Background technology
In recent years, as global industry process is constantly accelerated, problem of environmental pollution is increasingly serious, is increasingly becoming influence people
The major issue of the class survival and development.With the implementation and accession to WTO and the organic dirt of persistence of China's strategy of sustainable development
Dye thing（POPS）Pact, the pollution problem of organic pollution has turned into one of China's problem demanding prompt solution, therefore studies organic
Contaminant degradation new technology, to alleviating the increasingly serious environmental pressure of China and realizing that social sustainable development is significant.
Photocatalysis technology, i.e., carry out research of the Photocatalyst in terms of environmental improvement to pollutant using solar energy
It is more and more deep.Luminous energy can be converted into chemical energy by semi-conducting material under the irradiation of light, so as to promote the generation of compound
Or degraded, here it is photocatalysis technology.
Photocatalytic degradation treatment waste water technology is considered as to solve problem of environmental pollution most to have one of technology of application prospect,
The study hotspot of environmental area is turned into.Organic-inorganic hybrid material has good catalysis activity and selectivity, therefore, in recent years
Carry out the research that people have also concentrated one's gaze on sight hybrid inorganic-organic photochemical catalyst, and metal organic complex has energy of oxidation
Power is strong, degraded completely, energy consumption is low, the advantages of be readily synthesized recyclable with catalyst, cause the great interest of numerous researchers,
Also for environmental pollution improvement proposes new theory and approach.
The content of the invention
Present invention solves the technical problem that there is provided a kind of organic inorganic hybridization with photocatalytic activity in the sunlight
Material and preparation method thereof, the preparation method utilizes 1,2- bis- (4- picolines) ethane dibromo salt as cation template, leads to
Cross to be constructed with cuprous iodide self assembly and obtain organic-inorganic hybrid material, obtained organic-inorganic hybrid material to waste water in have
Engine dyeing material has preferable photocatalytic degradation effect.
The present invention is adopted the following technical scheme that to solve above-mentioned technical problem, a kind of to have photocatalytic activity in the sunlight
Organic-inorganic hybrid material, it is characterised in that its molecular formula is：C42H54Cu8I14N6, construction unit is：
。
The preparation method of the organic-inorganic hybrid material with photocatalytic activity in the sunlight of the present invention, its feature
It is to concretely comprise the following steps：（1）Cuprous iodide and KI are added to makes cuprous iodide-KI in dimethyl formamide solution
All dissolvings obtain solution A；（2）By 1,2- bis- (4- picolines), ethane dibromo salt is added to methanol solution is completely dissolved it
Obtain solution B；（3）Solution B is added drop-wise in solution A has pink precipitate to produce, and is added dropwise to complete rear filtering reacting liquid, and filtrate is quiet
Put, separate out pink acicular crystal after solvent flashing at room temperature, the acicular crystal uses distilled water and washes of absolute alcohol successively
The organic-inorganic hybrid material of target product cuprous iodide is dried to obtain afterwards.
Further limit, described 1,2- bis- (4- picolines) ethane dibromo salt, KI and cuprous iodide mole
Than being 1:4:1.
Further limit, step（1）The consumption of middle dimethyl formamide solution is 1mmol KIs correspondence dimethyl formyl
The volume of amine aqueous solution is 40mL.
Further limit, step（2）The consumption of middle methanol solution is 1mmol 1,2- bis- (4- picolines) ethane dibromo
The volume of salt correspondence methanol solution is 20mL.
Organic-inorganic hybrid material with photocatalytic activity in the sunlight of the present invention contains in photocatalytic degradation
Application in the organic wastewater of methyl orange, it is characterised in that concretely comprise the following steps：The organic wastewater that 100mL contains methyl orange is placed in
In beaker, the organic-inorganic hybrid material of 50mg cuprous iodides is added, simulate daylight with the xenon lamp of 500W, and filtered off with optical filter
Ultraviolet portion, the photocatalytic activity of methyl orange reaches more than 90% in organic wastewater after 3h.
The present invention has the advantages that compared with prior art：
1st, organic-inorganic hybrid material of the invention can be prepared by common natural volatility process technique, preparation method letter
Single easy, with low cost, energy saving, for the organic dyestuff in catalytic degradation waste water provides new selection, while expanding
The application value of organic-inorganic hybrid material；
2nd, organic-inorganic hybrid material stability of the invention is relatively good, is not decomposed substantially below 200 DEG C, keeps steady
It is fixed, and good activity is shown in the organic wastewater that photocatalytic degradation contains methyl orange, show that there is light very high to urge for it
Change activity and the feature of environmental protection.
Brief description of the drawings
Fig. 1 is the PXRD of the organic-inorganic hybrid material of cuprous iodide obtained in the embodiment of the present invention 1（X- powder diffractions
Figure）；
Fig. 2 is that the organic-inorganic hybrid material photocatalytic degradation of cuprous iodide obtained in the embodiment of the present invention 1 contains methyl
The absorbance change figure of the organic wastewater of orange；
Fig. 3 is the absorbance change figure that blank tests the organic wastewater containing methyl orange；
Fig. 4 is that the organic-inorganic hybrid material photocatalytic degradation of cuprous iodide obtained in the embodiment of the present invention 1 contains methyl
The change in concentration figure of the organic wastewater of orange.
Specific embodiment
The above of the invention is described in further details by the following examples, but this should not be interpreted as this
The scope for inventing above-mentioned theme is only limitted to following embodiment, and all technologies realized based on the above of the present invention belong to this hair
Bright scope.
Embodiment 1
The preparation of the organic-inorganic hybrid material of cuprous iodide
Cuprous iodide 19.1mg is weighed in the A vials of 10mL（0.1mmol）With KI 66.4mg（0.4mmol）,
Adding 4mL DMF solutions makes cuprous iodide-KI all dissolve；(the 4- methyl pyrroles of 1,2- bis- are weighed in the B vials of 7mL
Pyridine) ethane dibromo salt 37.4mg（0.1mmol）, add 2mL methanol solutions to be completely dissolved it；With suction pipe by the solution in B bottles
Dropwise it is added drop-wise in bottle A bottles, discovery there are a large amount of pink precipitates to produce, after solution is thoroughly mixed, is filled into one totally
Bottle in, stand, allow solvent volatilize naturally at room temperature, have the precipitation of pink acicular crystal after a few days, successively with distilled water with
Absolute ethanol washing, dries, and obtains the organic-inorganic hybrid material of target product cuprous iodide.Yield：86%（Calculated based on Cu
Obtain）.Every crystallographic parameter of the organic-inorganic hybrid material of cuprous iodide obtained in the present embodiment refers to table 1.
Every crystallographic parameter of the organic-inorganic hybrid material of the cuprous iodide of table 1
Embodiment 2
The preparation of the organic-inorganic hybrid material of cuprous iodide
Cuprous iodide 19.1mg is weighed in the A vials of 10mL（0.1mmol）With KI 66.4mg（0.4mmol）,
Adding 4mL DMF solutions makes cuprous iodide-KI all dissolve；(the 4- methyl pyrroles of 1,2- bis- are weighed in the B vials of 7mL
Pyridine) ethane dibromo salt 37.4mg（0.1mmol）, add 1mL methanol solutions to be completely dissolved it；With suction pipe by the solution in B bottles
Dropwise it is added drop-wise in bottle A bottles, discovery has a small amount of pink precipitate to produce, after solution is thoroughly mixed, is filled into one totally
Bottle in, stand, allow solvent volatilize naturally at room temperature, have the precipitation of pink acicular crystal after a few days, successively with distilled water with
Absolute ethanol washing, dries, and obtains the organic-inorganic hybrid material of target product cuprous iodide.Yield：63%（Calculated based on Cu
Obtain）.
Embodiment 3
The preparation of the organic-inorganic hybrid material of cuprous iodide
Cuprous iodide 19.1mg is weighed in the A vials of 10mL（0.1mmol）With KI 66.4mg（0.4 mmol）,
Adding 4mL DMF solutions makes cuprous iodide-KI all dissolve；(the 4- methyl pyrroles of 1,2- bis- are weighed in the B vials of 7mL
Pyridine) ethane dibromo salt 56.1mg（0.1mmol）, add 3mL methanol solutions to be completely dissolved it；With suction pipe by the solution in B bottles
Dropwise it is added drop-wise in bottle A bottles, discovery there are a large amount of pink precipitates to produce, after solution is thoroughly mixed, is filled into one totally
Bottle in, stand, allow solvent volatilize naturally at room temperature, have the precipitation of pink acicular crystal after a few days, successively with distilled water with
Absolute ethanol washing, dries, and obtains the organic-inorganic hybrid material of target product cuprous iodide.Yield：41%（Calculated based on Cu
Obtain）.
Embodiment 4
The organic-inorganic hybrid material photocatalytic degradation of cuprous iodide prepared by embodiment 1 contains the organic wastewater of methyl orange
It is 5.0 × 10 to prepare molar concentration first-5The methyl orange of mol/L（MO）Solution 100mL, weighs 50mg embodiments 1
The organic-inorganic hybrid material of obtained cuprous iodide is added in MO solution as photochemical catalyst, in order to ensure adsorption equilibrium,
Dark place magnetic agitation 30min, then simulates daylight with the xenon lamp of 500W, and filters off ultraviolet portion with optical filter, is not added with any
The MO solution of catalyst does blank control test, at interval of 30min, takes 3mL solution and is analyzed, and does the UV absorption light of solution
Spectrum, as shown in Figures 2 and 3, is then concentration proportion C/C again0To the curve of time t（C 0 It is the initial concentration of MO solution, when C is
Between for t when MO solution concentration), as shown in Figure 4.
Embodiment above describes general principle of the invention, principal character and advantage, the technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, simply original of the invention is illustrated described in above-described embodiment and specification
Reason, under the scope for not departing from the principle of the invention, various changes and modifications of the present invention are possible, and these changes and improvements each fall within
In the scope of protection of the invention.
Claims (7)
1. a kind of organic-inorganic hybrid material with photocatalytic activity in the sunlight, it is characterised in that its molecular formula is：
C42H54Cu8I14N6, construction unit is：
。
2. described in a kind of claim 1 in the sunlight with photocatalytic activity organic-inorganic hybrid material preparation method,
It is characterized in that concretely comprising the following steps：（1）Cuprous iodide and KI are added in dimethyl formamide solution make cuprous iodide-
All dissolving obtains solution A to KI；（2）By 1,2- bis- (4- picolines), ethane dibromo salt is added to methanol solution makes its complete
CL obtains solution B；（3）Solution B is added drop-wise in solution A has pink precipitate to produce, and is added dropwise to complete rear filtering reacting liquid,
Filtrate stands, and separates out pink acicular crystal after solvent flashing at room temperature, and the acicular crystal uses distilled water and anhydrous second successively
The organic-inorganic hybrid material of target product cuprous iodide is dried to obtain after alcohol cleaning.
3. it is according to claim 2 in the sunlight with photocatalytic activity organic-inorganic hybrid material preparation method,
It is characterized in that：The mol ratio of described 1,2- bis- (4- picolines) ethane dibromo salt, KI and cuprous iodide is 1:4:
1。
4. it is according to claim 2 in the sunlight with photocatalytic activity organic-inorganic hybrid material preparation method,
It is characterized in that：Step（1）The consumption of middle dimethyl formamide solution is 1mmol KIs correspondence dimethyl formamide solution
Volume is 40mL.
5. it is according to claim 2 in the sunlight with photocatalytic activity organic-inorganic hybrid material preparation method,
It is characterized in that：Step（2）The consumption of middle methanol solution is 1mmol 1,2- bis- (4- picolines) ethane dibromo salt correspondence first
The volume of alcoholic solution is 20mL.
6. the organic-inorganic hybrid material with photocatalytic activity in the sunlight described in claim 1 contains in photocatalytic degradation
Application in the organic wastewater of methyl orange.
7. the organic-inorganic hybrid material with photocatalytic activity in the sunlight according to claim 6 is in photocatalytic degradation
Application in organic wastewater containing methyl orange, it is characterised in that concretely comprise the following steps：100mL is contained the organic wastewater of methyl orange
It is placed in beaker, adds the organic-inorganic hybrid material of 50mg cuprous iodides, simulates daylight with the xenon lamp of 500W, and use optical filter
Ultraviolet portion is filtered off, the photocatalytic activity of methyl orange reaches more than 90% in organic wastewater after 3h.
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| CN112426987A (en) * | 2020-12-28 | 2021-03-02 | 北京大学深圳研究生院 | Ceramic vessel with inner wall doped with photocatalytic material |
| CN112898961B (en) * | 2021-01-25 | 2022-11-25 | 深圳大学 | Organic-inorganic hybrid scintillator and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011240340A (en) * | 2006-12-13 | 2011-12-01 | Korea Res Inst Of Chem Technol | Porous organic-inorganic hybrid material, and adsorbent containing the same |
| CN102698807A (en) * | 2012-07-03 | 2012-10-03 | 昆明理工大学 | Noble metal nano catalyst prepared from organic azo dyes functionalized carbon nano materials and preparation method of catalyst |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011240340A (en) * | 2006-12-13 | 2011-12-01 | Korea Res Inst Of Chem Technol | Porous organic-inorganic hybrid material, and adsorbent containing the same |
| CN102698807A (en) * | 2012-07-03 | 2012-10-03 | 昆明理工大学 | Noble metal nano catalyst prepared from organic azo dyes functionalized carbon nano materials and preparation method of catalyst |
Non-Patent Citations (1)
| Title |
|---|
| Synthesis, structure and photocatalytic properties of two novel Ag(I) polymers directed by 1,3-bis(4-methylpyridine)alkane cation;Mei Liu，et al;《J Clust Sci》;20150312;第26卷;全文 * |
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