CN105289752A - Organic-inorganic hybrid material with photocatalytic activity in sunlight, and preparation method and application of organic-inorganic hybrid material - Google Patents
Organic-inorganic hybrid material with photocatalytic activity in sunlight, and preparation method and application of organic-inorganic hybrid material Download PDFInfo
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- CN105289752A CN105289752A CN201510588254.4A CN201510588254A CN105289752A CN 105289752 A CN105289752 A CN 105289752A CN 201510588254 A CN201510588254 A CN 201510588254A CN 105289752 A CN105289752 A CN 105289752A
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Abstract
The invention discloses an organic-inorganic hybrid material with photocatalytic activity in the sunlight, and a preparation method and application of the organic-inorganic hybrid material. A molecular formula of the organic-inorganic hybrid material is C42H54Cu8I14N6; a structural unit is shown in the specification; positive ions are dissolved with a methanol solution; a metal salt is dissolved with a Dimethyl Formamide (DMF) solution; the ratio of the positive ions to the metal salt is adjusted to obtain a nearly saturated solution; the nearly saturated solution is filtered by filter paper to obtain clear liquid; the organic-inorganic hybrid material of a target product copper iodide is obtained by standing and volatilizing a solvent. The preparation method disclosed by the invention is simple and feasible; the prepared organic-inorganic hybrid material is high in stability, is basically not decomposed below 200 DEG C, is kept stable, and shows very high activity in photocatalytic degradation of methyl orange-containing organic wastewater.
Description
Technical field
The invention belongs to catalysis material technical field, be specifically related to a kind of organic-inorganic hybrid material with photocatalytic activity in the sunlight and its preparation method and application.
Background technology
In recent years, along with global industry process is constantly accelerated, problem of environmental pollution is day by day serious, becomes the major issue affecting human survival and development gradually.Along with China's strategy of sustainable development enforcement and accession to WTO and persistence organic pollutant (POPS) pact, the pollution problem of organic pollution has become one of China's problem demanding prompt solution, therefore organic pollutant degradation new technology is studied, significant to alleviating the increasingly serious environmental pressure of China and realizing social sustainable development.
Photocatalysis technology, namely utilizes solar energy to carry out the research of Photocatalyst in environmental improvement to pollutant more and more deep.Semi-conducting material can be chemical energy light energy conversion under the irradiation of light, thus promotes the generation of compound or degraded, Here it is photocatalysis technology.
Photocatalytic degradation process waste water technology is considered to solve problem of environmental pollution most one of technology having application prospect, becomes the study hotspot of environmental area.Organic-inorganic hybrid material has good catalytic activity and selective, therefore, people have also concentrated one's gaze on sight the research of hybrid inorganic-organic photochemical catalyst in recent years, and metal organic complex has that oxidability is strong, degraded completely, the advantage such as energy consumption is low, be easy to synthesis and catalyst is recyclable, cause the great interest of numerous researchers, also for environmental pollution improvement proposes new theory and approach.
Summary of the invention
The technical problem that the present invention solves there is provided a kind of organic-inorganic hybrid material with photocatalytic activity in the sunlight and preparation method thereof, this preparation method utilizes 1,2-bis-(4-picoline) ethane dibromo salt is as cation template, obtain organic-inorganic hybrid material by constructing with cuprous iodide self assembly, obtained organic-inorganic hybrid material has good photocatalytic degradation effect to the organic dyestuff in waste water.
The present invention adopts following technical scheme for solving the problems of the technologies described above, and a kind of organic-inorganic hybrid material in the sunlight with photocatalytic activity, is characterized in that its molecular formula is: C
42h
54cu
8i
14n
6, construction unit is:
。
The preparation method in the sunlight with the organic-inorganic hybrid material of photocatalytic activity of the present invention, is characterized in that concrete steps are: cuprous iodide and KI join in dimethyl formamide solution and cuprous iodide-KI all dissolved obtain solution A by (1); (2) 1,2-bis-(4-picoline) ethane dibromo salt is joined methanol solution to make it dissolve completely to obtain solution B; (3) solution B is added drop-wise in solution A there is pink precipitate to produce, be added dropwise to complete rear filtering reacting liquid, filtrate leaves standstill, under room temperature, separate out pink acicular crystal after solvent flashing, this acicular crystal is successively with the organic-inorganic hybrid material obtaining target product cuprous iodide dry after distilled water and washes of absolute alcohol.
Further restriction, the mol ratio of described 1,2-bis-(4-picoline) ethane dibromo salt, KI and cuprous iodide is 1:4:1.
Further restriction, in step (1), the consumption of dimethyl formamide solution is the volume of the corresponding dimethyl formamide solution of 1mmol KI is 40mL.
Further restriction, in step (2), the consumption of methanol solution is the volume of the corresponding methanol solution of 1mmol1,2-bis-(4-picoline) ethane dibromo salt is 20mL.
The organic-inorganic hybrid material in the sunlight with photocatalytic activity of the present invention contains the application in the organic wastewater of methyl orange at photocatalytic degradation, it is characterized in that concrete steps are: organic wastewater 100mL being contained methyl orange is placed in beaker, add the organic-inorganic hybrid material of 50mg cuprous iodide, by the xenon lamp solar simulated of 500W, and with optical filter elimination ultraviolet portion, after 3h, in organic wastewater, the photocatalytic activity of methyl orange reaches more than 90%.
The present invention compared with prior art has following beneficial effect:
1, organic-inorganic hybrid material of the present invention can by common natural volatility process technique preparation, preparation method is simple, with low cost, economize energy, for the organic dyestuff in catalytic degradation waste water provides new selection, expanded the using value of organic-inorganic hybrid material simultaneously;
2, organic-inorganic hybrid material stability of the present invention is relatively good, substantially do not decompose below 200 DEG C, keep stable, and contain at photocatalytic degradation in the organic wastewater of methyl orange and show good activity, show that it has very high photocatalytic activity and the feature of environmental protection.
Accompanying drawing explanation
Fig. 1 is the PXRD(X-powder diagram of the organic-inorganic hybrid material of the cuprous iodide that the embodiment of the present invention 1 obtains);
Fig. 2 is the absorbance variation diagram that the organic-inorganic hybrid material photocatalytic degradation of the obtained cuprous iodide of the embodiment of the present invention 1 contains the organic wastewater of methyl orange;
Fig. 3 is the absorbance variation diagram of the organic wastewater of blank experiment containing methyl orange;
Fig. 4 is the change in concentration figure that the organic-inorganic hybrid material photocatalytic degradation of the obtained cuprous iodide of the embodiment of the present invention 1 contains the organic wastewater of methyl orange.
Detailed description of the invention
Be described in further details foregoing of the present invention by the following examples, but this should be interpreted as that the scope of the above-mentioned theme of the present invention is only limitted to following embodiment, all technology realized based on foregoing of the present invention all belong to scope of the present invention.
Embodiment 1
The preparation of the organic-inorganic hybrid material of cuprous iodide
Cuprous iodide 19.1mg(0.1mmol is taken in the A vial of 10mL) and KI 66.4mg(0.4mmol), add 4mLDMF solution and cuprous iodide-KI is all dissolved; 1,2-bis-(4-picoline) ethane dibromo salt 37.4mg(0.1mmol is taken in the B vial of 7mL), add 2mL methanol solution and make it dissolve completely; With suction pipe, the dropwise in B bottle is added drop-wise in bottle A bottle, find that there is a large amount of pink precipitate to produce, after solution mixes completely, be filled in a clean bottle, leave standstill, under room temperature, allow solvent naturally volatilize, pink acicular crystal is had to separate out after several days, use distilled water and absolute ethanol washing successively, dry, obtain the organic-inorganic hybrid material of target product cuprous iodide.Productive rate: 86%(calculates based on Cu).Every crystallographic parameter of the organic-inorganic hybrid material of the cuprous iodide that the present embodiment obtains refers to table 1.
Every crystallographic parameter of the organic-inorganic hybrid material of table 1 cuprous iodide
Embodiment 2
The preparation of the organic-inorganic hybrid material of cuprous iodide
Cuprous iodide 19.1mg(0.1mmol is taken in the A vial of 10mL) and KI 66.4mg(0.4mmol), add 4mLDMF solution and cuprous iodide-KI is all dissolved; 1,2-bis-(4-picoline) ethane dibromo salt 37.4mg(0.1mmol is taken in the B vial of 7mL), add 1mL methanol solution and make it dissolve completely; With suction pipe, the dropwise in B bottle is added drop-wise in bottle A bottle, find that there is a small amount of pink precipitate to produce, after solution mixes completely, be filled in a clean bottle, leave standstill, under room temperature, allow solvent naturally volatilize, pink acicular crystal is had to separate out after several days, use distilled water and absolute ethanol washing successively, dry, obtain the organic-inorganic hybrid material of target product cuprous iodide.Productive rate: 63%(calculates based on Cu).
Embodiment 3
The preparation of the organic-inorganic hybrid material of cuprous iodide
Cuprous iodide 19.1mg(0.1mmol is taken in the A vial of 10mL) and KI 66.4mg(0.4mmol), add 4mLDMF solution and cuprous iodide-KI is all dissolved; 1,2-bis-(4-picoline) ethane dibromo salt 56.1mg(0.1mmol is taken in the B vial of 7mL), add 3mL methanol solution and make it dissolve completely; With suction pipe, the dropwise in B bottle is added drop-wise in bottle A bottle, find that there is a large amount of pink precipitate to produce, after solution mixes completely, be filled in a clean bottle, leave standstill, under room temperature, allow solvent naturally volatilize, pink acicular crystal is had to separate out after several days, use distilled water and absolute ethanol washing successively, dry, obtain the organic-inorganic hybrid material of target product cuprous iodide.Productive rate: 41%(calculates based on Cu).
Embodiment 4
The organic-inorganic hybrid material photocatalytic degradation of cuprous iodide prepared by embodiment 1 contains the organic wastewater of methyl orange
First preparing molar concentration is 5.0 × 10
-5methyl orange (MO) the solution 100mL of mol/L, the organic-inorganic hybrid material taking the obtained cuprous iodide of 50mg embodiment 1 joins in MO solution as photochemical catalyst, in order to ensure adsorption equilibrium, dark place magnetic agitation 30min, then the xenon lamp solar simulated of 500W is used, and with optical filter elimination ultraviolet portion, the MO solution not adding any catalyst does blank test, at interval of 30min, get 3mL solution to analyze, do the ultra-violet absorption spectrum of solution, as shown in Figures 2 and 3, and then do concentration proportion
c/C 0 to the curve of time t (
c 0 for the initial concentration of MO solution,
cthe concentration of MO solution when be the time being t), as shown in Figure 4.
Embodiment above describes general principle of the present invention, principal character and advantage; the technical staff of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and description just illustrates principle of the present invention; under the scope not departing from the principle of the invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the scope of protection of the invention.
Claims (7)
1. there is an organic-inorganic hybrid material for photocatalytic activity in the sunlight, it is characterized in that its molecular formula is: C
42h
54cu
8i
14n
6, construction unit is:
。
2. a preparation method in the sunlight with the organic-inorganic hybrid material of photocatalytic activity according to claim 1, is characterized in that concrete steps are: cuprous iodide and KI join in dimethyl formamide solution and cuprous iodide-KI all dissolved obtain solution A by (1); (2) 1,2-bis-(4-picoline) ethane dibromo salt is joined methanol solution to make it dissolve completely to obtain solution B; (3) solution B is added drop-wise in solution A there is pink precipitate to produce, be added dropwise to complete rear filtering reacting liquid, filtrate leaves standstill, under room temperature, separate out pink acicular crystal after solvent flashing, this acicular crystal is successively with the organic-inorganic hybrid material obtaining target product cuprous iodide dry after distilled water and washes of absolute alcohol.
3. the preparation method in the sunlight with the organic-inorganic hybrid material of photocatalytic activity according to claim 1, it is characterized in that: the mol ratio of described 1,2-bis-(4-picoline) ethane dibromo salt, KI and cuprous iodide is 1:4:1.
4. the preparation method in the sunlight with the organic-inorganic hybrid material of photocatalytic activity according to claim 1, is characterized in that: in step (1), the consumption of dimethyl formamide solution is the volume of the corresponding dimethyl formamide solution of 1mmol KI is 40mL.
5. the preparation method in the sunlight with the organic-inorganic hybrid material of photocatalytic activity according to claim 1, it is characterized in that: in step (2), the consumption of methanol solution is the volume of the corresponding methanol solution of 1mmol1,2-bis-(4-picoline) ethane dibromo salt is 20mL.
6. the organic-inorganic hybrid material in the sunlight with photocatalytic activity according to claim 1 contains the application in the organic wastewater of methyl orange at photocatalytic degradation.
7. the organic-inorganic hybrid material in the sunlight with photocatalytic activity according to claim 6 contains the application in the organic wastewater of methyl orange at photocatalytic degradation, it is characterized in that concrete steps are: organic wastewater 100mL being contained methyl orange is placed in beaker, add the organic-inorganic hybrid material of 50mg cuprous iodide, by the xenon lamp solar simulated of 500W, and with optical filter elimination ultraviolet portion, after 3h, in organic wastewater, the photocatalytic activity of methyl orange reaches more than 90%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN112898961A (en) * | 2021-01-25 | 2021-06-04 | 深圳大学 | Organic-inorganic hybrid scintillator and preparation method and application thereof |
Citations (2)
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|---|---|---|---|---|
| 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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Patent 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 |
Non-Patent Citations (1)
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| MEI LIU，ET AL: "Synthesis, structure and photocatalytic properties of two novel Ag(I) polymers directed by 1,3-bis(4-methylpyridine)alkane cation", 《J CLUST SCI》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN112898961A (en) * | 2021-01-25 | 2021-06-04 | 深圳大学 | Organic-inorganic hybrid scintillator and preparation method and application thereof |
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