CN106582719A - Preparation method for CdS/MIL-53 (Fe) visible light catalyst - Google Patents
Preparation method for CdS/MIL-53 (Fe) visible light catalyst Download PDFInfo
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- CN106582719A CN106582719A CN201610931647.5A CN201610931647A CN106582719A CN 106582719 A CN106582719 A CN 106582719A CN 201610931647 A CN201610931647 A CN 201610931647A CN 106582719 A CN106582719 A CN 106582719A
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- cds
- visible light
- polyvinylpyrrolidone
- thioacetamide
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- 239000013206 MIL-53 Substances 0.000 title claims abstract description 74
- 239000003054 catalyst Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 72
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000000463 material Substances 0.000 claims abstract description 28
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 27
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 27
- LHQLJMJLROMYRN-UHFFFAOYSA-L cadmium acetate Chemical compound [Cd+2].CC([O-])=O.CC([O-])=O LHQLJMJLROMYRN-UHFFFAOYSA-L 0.000 claims abstract description 26
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 23
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 22
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims abstract description 19
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000005119 centrifugation Methods 0.000 claims abstract description 7
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 17
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 239000002131 composite material Substances 0.000 claims description 12
- 230000008859 change Effects 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 7
- 239000000376 reactant Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- 238000013019 agitation Methods 0.000 claims description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 3
- GNFTZDOKVXKIBK-UHFFFAOYSA-N 3-(2-methoxyethoxy)benzohydrazide Chemical compound COCCOC1=CC=CC(C(=O)NN)=C1 GNFTZDOKVXKIBK-UHFFFAOYSA-N 0.000 claims description 2
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 claims description 2
- HUKFCVYEXPZJJZ-UHFFFAOYSA-N cadmium;hydrate Chemical compound O.[Cd] HUKFCVYEXPZJJZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000013461 design Methods 0.000 claims description 2
- 238000004821 distillation Methods 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims 1
- 239000000243 solution Substances 0.000 claims 1
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 abstract description 39
- 229910052980 cadmium sulfide Inorganic materials 0.000 abstract description 39
- 230000003197 catalytic effect Effects 0.000 abstract description 10
- 238000006731 degradation reaction Methods 0.000 abstract description 9
- 230000015556 catabolic process Effects 0.000 abstract description 8
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 abstract description 8
- 229940043267 rhodamine b Drugs 0.000 abstract description 8
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 239000012153 distilled water Substances 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract 1
- 238000004729 solvothermal method Methods 0.000 abstract 1
- 239000012621 metal-organic framework Substances 0.000 description 8
- 230000001699 photocatalysis Effects 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 6
- 230000006872 improvement Effects 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000000725 suspension Substances 0.000 description 4
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 230000004044 response Effects 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- SCVJRXQHFJXZFZ-KVQBGUIXSA-N 2-amino-9-[(2r,4s,5r)-4-hydroxy-5-(hydroxymethyl)oxolan-2-yl]-3h-purine-6-thione Chemical compound C1=2NC(N)=NC(=S)C=2N=CN1[C@H]1C[C@H](O)[C@@H](CO)O1 SCVJRXQHFJXZFZ-KVQBGUIXSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 150000001408 amides Chemical class 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- ZSDJVGXBJDDOCD-UHFFFAOYSA-N benzene dioctyl benzene-1,2-dicarboxylate Chemical compound C(C=1C(C(=O)OCCCCCCCC)=CC=CC1)(=O)OCCCCCCCC.C1=CC=CC=C1 ZSDJVGXBJDDOCD-UHFFFAOYSA-N 0.000 description 2
- 229910052793 cadmium Inorganic materials 0.000 description 2
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000010025 steaming Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 239000013265 porous functional material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/043—Sulfides with iron group metals or platinum group metals
-
- B01J35/39—
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
Abstract
The invention relates to a preparation method for a novel CdS/MIL-53 (Fe) visible light catalyst. The preparation method comprises the steps that an MIL-53 (Fe) material is prepared from ferric trichloride, terephthalic acid and N,N-dimethylformamide at the molar ratio of 1:1:65 by adopting the solvothermal method at first; then cadmium acetate, thioacetamide, polyvinylpyrrolidone, ethylene glycol and MIL-53 (Fe) are weighed according to the mass ratio of cadmium sulfide to the MIL-53 (Fe) being (1-1.5):1, and the MIL-53 (Fe) is dispersed in the ethylene glycol; the cadmium acetate is added; and the thioacetamide and the polyvinylpyrrolidone are added, reaction is conducted for 12 hours at the temperature of 180 DEG C, centrifugation, secondary distilled water washing and absolute ethyl alcohol washing are conducted for 5-6 times, drying is conducted for 10 hours at the temperature of 60 DEG C, and the CdS/MIL-53 (Fe) visible light catalyst is finally obtained. The catalytic activity of the CdS/MIL-53 (Fe) visible light catalyst is excellent, and the degradation rate of the visible light catalyst on rhodamine B is 71%-90%.
Description
Technical field
The present invention relates to the method that one kind prepares CdS/MIL-53 (Fe) visible light catalyst, the material is urged for visible ray
Change the organic pollutions such as rhodamine B degradation, belong to catalysis material preparing technical field.
Background technology
Photocatalysis technology as a kind of novel environmental close friend's catalysis technique, in environmental improvement, new energy development and organic
The application in the fields such as synthesis is of increasing concern.Especially in environmental improvement side and, Photocatalyst is being increasingly becoming biography
The system supplement of pollutant abatement technology and perfect.Its maximum advantage is that degradation reaction is typically carried out at normal temperatures and pressures, energy
Thoroughly decompose water body and the organic pollution in air so as to which mineralising is CO2And H2O.Additionally, photocatalysis technology is to utilize luminous energy,
Compared with other traditional pollutant abatement technologies, the use of other energy can be saved, alleviate increasingly serious energy crisis.
The energy gap of cadmium sulfide (CdS) is 2.4 eV, with good visible absorption response and photohole electricity
The redox ability of son, can be used for organic molecular group of degrading.CdS preparation methoies are simple, it is easy to nanorize, and crystallinity
Good, these features cause CdS to have the performance of good photocatalytic degradation Organic substance.But CdS nano-particle is easy to reunite, in light
Catalytic process can not be contacted fully with organic pollution so that rate of photocatalytic oxidation is reduced.
Metal-organic framework materials（metal-organic frameworks, MOFs）Be it is a kind of it is new, with receiving
The porous functional material of micro structure, the specific surface area with superelevation and pore volume, open pore structure, homogeneous pore-size distribution, no
The metal-complexing of saturation, adjustable pore structure and surface property, and thousands of kinds of species of various fit systems composition, this
A little excellent characteristics all cause MOFs all to have great potentiality in terms of scientific research or commercial Application.In recent years
Research shows there is the features such as the specific surface area of adjustable pore structure, superelevation just because of MOFs, with traditional visible ray
Material is compared, and MOFs materials show good visible light-responded performance.Wherein MIL-53 (Fe)（P-phthalic acid ferrum）It is one
Plant metal ion, the MOF being made up of octahedra Fe (III) and Isosorbide-5-Nitrae-p-phthalic acid chain, its forbidden band centered on Fe (III)
Width is 2.82 eV, is a kind of MOF materials containing Fe (III), with it is nontoxic, stable, inexpensively and to the spy such as visible light-responded
Point.
There are some researches show that can improve material by the method for composite semiconductor material urges the absorption of light and visible ray
Change performance, so as to improve the Photocatalytic Activity for Degradation efficiency of material.Solvent-thermal method leads to as a kind of " chemical process of soft solution "
Overregulating the condition of solvent thermal reaction can control the size and pattern of crystal grain, change microstructure, phase composition and the change of material
Learn property.
Jing is retrieved, and is not found with cadmium acetate, thioacetamide and MIL-53 (Fe) as raw material, using solvent thermal technology, system
The patent application of the method for standby novel C dS/MIL-53 (Fe) visible light catalytic material and document report.The purpose of the present invention is logical
Cross solvent-thermal method to prepare CdS/MIL-53 (Fe) composite, make both forbidden bands obtain coupling so as to widen whole composite wood
Response range of the material to visible ray, increases the photocatalytic activity under its visible ray；By the quality for controlling CdS and MIL-53 (Fe)
Than preparing not
CdS/MIL-53 (Fe) in proportion, so as to provide a kind of visible light catalyst composite.
The content of the invention
The purpose of the present invention is：Visible light catalyst CdS/ is obtained by controlling the mass ratio of CdS and MIL-53 (Fe)
MIL-53 (Fe), and the degradation effect to rhodamine B reaches most preferably.
To realize the present invention, technical scheme is as follows：
A kind of preparation method of CdS/MIL-53 (Fe) visible light catalyst, it is characterised in that with following process and step：
A. MIL-53 (Fe) is prepared
A. ferric chloride is pressed：P-phthalic acid：N,N-dimethylformamide=1：1：The ratio of 65 (mol ratios) weighs respectively trichlorine
Change ferrum, p-phthalic acid, N,N-dimethylformamide；
Described ferric chloride is ferric chloride (FeCl36H2O)；
B. the ferric chloride weighed by step a, p-phthalic acid are dissolved in DMF, are fully stirred at room temperature
Mix, ferric chloride, p-phthalic acid is fully dissolved, DMF of the configuration containing ferric chloride and p-phthalic acid
Solution；
C. the N,N-dimethylformamide solution containing ferric chloride and p-phthalic acid configured by step b is moved into into 100mL
Reactor in, reactor is put in 150 DEG C of baking oven, react 12 hours, after being cooled to room temperature, centrifugation must react
Thing；
D. will be washed with redistilled water and absolute methanol 5 ~ 6 times by step c gained reactant, place into 500 mL second distillations
The night of agitator treating one obtains washings in water；Washings are dried 10 hours at 60 DEG C, product MIL-53 (Fe) is obtained.
B. CdS is produced by cadmium acetate, thioacetamide, and CdS/MIL-53 (Fe) composite is further obtained
A. formula design requirement, CdS are pressed:MIL-53(Fe)=(1~1.5):1（Mass ratio）Calculated, taken each participation raw material
The expense of material；
B. cadmium acetate is pressed：Thioacetamide=1:The ratio of 1 (mol ratios) weighs respectively cadmium acetate and thioacetamide；
Described cadmium acetate is two water cadmium acetates；
C. polyvinylpyrrolidone is pressed：Ethylene glycol=0.2:The ratio of 100 (g/mL) weighs respectively polyvinylpyrrolidone and second two
Alcohol；
Described polyvinylpyrrolidone is PVP K-30；
D., during the MIL-53 (Fe) weighed by step a to be scattered in the 100 mL ethylene glycol measured by step c, magnetic force is stirred under room temperature
Mix, make MIL-53 (Fe) fully dispersed；
E. the cadmium acetate weighed by step b is dissolved in the mixed liquor of the ethylene glycol containing MIL-53 (Fe) prepared by step d, room
The lower magnetic agitation of temperature, makes cadmium acetate fully dissolve；
F. the polyvinylpyrrolidone for weighing by the thioacetamide weighed by step b and by step c is dissolved in jointly is matched somebody with somebody by step e
In the mixed liquor of system, magnetic agitation under room temperature makes thioacetamide and polyvinylpyrrolidone fully dissolve；
G. by the ethylene glycol containing MIL-53 (Fe), cadmium acetate, thioacetamide and polyvinylpyrrolidone prepared by step f
Mixed liquor is moved in the reactor of 150 mL, and reactor is put in 180 DEG C of baking oven, is reacted 12 hours, is cooled to room
Wen Hou, centrifugation obtains reactant；
H. by the reactant redistilled water as obtained by step g and absolute ethanol washing 5 ~ 6 times, washings are obtained；By washings
It is dried at 60 DEG C 10 hours, CdS/MIL-53 (Fe) visible light catalyst composite products is finally obtained.
The present invention principle be：Cadmium acetate is dissolved in ethylene glycol can discharge Cd2+, Cd2+It is dispersed under stirring
In the surface of MIL-53 (Fe) or internal void；Thioacetamide is dissolved in after ethylene glycol can discharge S2-。Cd2+Easily with S2-Instead
CdS core should be generated.CdS core is uniformly distributed in the surface of MIL-53 (Fe) in the presence of surfactant polyvinylpyrrolidone
In hole.With the prolongation in response time, CdS core is grown into, and crystallite dimension also gradually increases.The Jing solvent thermal of 12 hours
Reaction has ultimately produced CdS/MIL-53 (Fe) visible light catalyst.
Description of the drawings
Fig. 1 is the XRD figure of CdS/MIL-53 (Fe) visible light catalytic material that embodiment 1 and example 2 are obtained；Wherein a is generation
The XRD curves of CdS/MIL-53 (Fe) visible light catalytic material that table embodiment 1 is obtained, b is the CdS/ for representing the acquisition of embodiment 2
The XRD curves of MIL-53 (Fe) visible light catalytic material.
Fig. 2 is the SEM figures of CdS/MIL-53 (Fe) visible light catalytic material that embodiment 1 is obtained.
Fig. 3 is CdS/MIL-53 (Fe) visible light catalytic material that obtains of embodiment 1 and example 2 under visible light illumination to sieve
The degradation rate figure of red bright B；Wherein a is CdS/MIL-53 (Fe) visible light catalytic material for representing the acquisition of embodiment 1 to rhodamine B
Degradation curve, b be represent the acquisition of embodiment 2 CdS/MIL-53 (Fe) visible light catalytic materials it is bent to the degraded of rhodamine B
Line.
Specific embodiment
With reference to embodiment and accompanying drawing, the present invention will be further explained.
Embodiment 1
The present embodiment is comprised the following steps that：
In the present embodiment, the preparation method of CdS/MIL-53 (Fe) visible light catalyst, the method is first with ferric chloride, to benzene
Dioctyl phthalate and DMF are raw material, and using solvent-thermal method MIL-53 (Fe) material is prepared；Again with the MIL- of gained
53 (Fe) and cadmium acetate, thioacetamide, polyvinylpyrrolidone and ethylene glycol are raw material, and using solvent-thermal method CdS/ is prepared
MIL-53 (Fe) composite.Its technical process is：Weigh the FeCl of 10 mmol3·6H2The p-phthalic acid of O and 10 mmol
In being dissolved in the DMF reagent of 50 mL jointly, it is stirred continuously at room temperature, makes ferric chloride and p-phthalic acid
Fully dissolving；Gained mixed liquor is moved in 100 mL reactors, reactor is put in 150 DEG C of baking oven, reacted 12 hours；
After being cooled to room temperature, it is centrifuged, after redistilled water and absolute methanol wash 5 ~ 6 times, places into 500 mL, bis- steamings
It is stirred overnight in distilled water；After recentrifuge, MIL-53 (Fe) material is dried 10 hours to obtain at 60 DEG C.Weigh obtained by 0.50 g
MIL-53 (Fe) material, add 100 mL ethylene glycol in, be stirred continuously under room temperature, make MIL-53 (Fe) be uniformly dispersed；Weigh
1.38 g Cd(CH3COO)2·2H2O, in adding the ethylene glycol suspension containing MIL-53 (Fe), is sufficiently stirred under room temperature, makes second
Sour cadmium fully dissolves；0.39 g thioacetamides and 0.20 g polyvinylpyrrolidones are weighed, is added containing cadmium acetate and MIL-
In the ethylene glycol suspension of 53 (Fe), it is sufficiently stirred under room temperature, thioacetamide and polyvinylpyrrolidone is fully dissolved, matches somebody with somebody
Make the mixed liquor of the ethylene glycol containing thioacetamide, polyvinylpyrrolidone, cadmium acetate and MIL-53 (Fe)；Thio second will be contained
The mixed liquor of the ethylene glycol of amide, polyvinylpyrrolidone, cadmium acetate and MIL-53 (Fe) is moved in the reactor of 200 mL,
Reactor is put in 180 DEG C of baking oven, is reacted 12 hours, to be cooled to after room temperature, Jing centrifugations, redistilled water and anhydrous second
Alcohol washs 5 ~ 6 times, is dried 10 hours at 60 DEG C, and CdS/MIL-53 (Fe) visible light catalyst composite products are finally obtained.
With novel C dS/MIL-53 (Fe) visible light catalyst Jing X-ray diffraction analysis prepared by above-mentioned processing step（Figure
1a）, consisting of CdS and MIL-53 (Fe).Scanned testing electronic microscope analyzes (Fig. 2), and its pattern is spherical, average grain
Footpath is 10 nm.Jing Visible Light Induced Photocatalytic rhodamine B solution testing analysis shows（Fig. 3 a）, its degradation rate to rhodamine B solution is
90%。
CdS/MIL-53 (Fe) visible light catalyst prepared by the present invention can be widely applied to environmental pollution improvement and light is urged
Change chemical field.
Embodiment 2
The present embodiment is comprised the following steps that：
In the present embodiment, the preparation method of CdS/MIL-53 (Fe) visible light catalyst, the method is first with ferric chloride, to benzene
Dioctyl phthalate and DMF are raw material, and using solvent-thermal method MIL-53 (Fe) material is prepared；Again with the MIL- of gained
53 (Fe) and cadmium acetate, thioacetamide, polyvinylpyrrolidone and ethylene glycol are raw material, and using solvent-thermal method CdS/ is prepared
MIL-53 (Fe) composite.Its technical process is：Weigh the FeCl of 10 mmol3·6H2The p-phthalic acid of O and 10 mmol
In being dissolved in the DMF reagent of 50 mL jointly, it is stirred continuously at room temperature, makes ferric chloride and p-phthalic acid
Fully dissolving；Gained mixed liquor is moved in 100 mL reactors, reactor is put in 150 DEG C of baking oven, reacted 12 hours；
After being cooled to room temperature, it is centrifuged, after redistilled water and absolute methanol wash 5 ~ 6 times, places into 500 mL, bis- steamings
It is stirred overnight in distilled water；After recentrifuge, MIL-53 (Fe) material is dried 10 hours to obtain at 60 DEG C.Weigh obtained by 0.50 g
MIL-53 (Fe) material, add 100 mL ethylene glycol in, be stirred continuously under room temperature, make MIL-53 (Fe) be uniformly dispersed；Weigh
0.92 g Cd(CH3COO)2·2H2O, in adding the ethylene glycol suspension containing MIL-53 (Fe), is sufficiently stirred under room temperature, makes second
Sour cadmium fully dissolves；0.26 g thioacetamides and 0.20 g polyvinylpyrrolidones are weighed, is added containing cadmium acetate and MIL-
In the ethylene glycol suspension of 53 (Fe), it is sufficiently stirred under room temperature, thioacetamide and polyvinylpyrrolidone is fully dissolved, matches somebody with somebody
Make the mixed liquor of the ethylene glycol containing thioacetamide, polyvinylpyrrolidone, cadmium acetate and MIL-53 (Fe)；Thio second will be contained
The mixed liquor of the ethylene glycol of amide, polyvinylpyrrolidone, cadmium acetate and MIL-53 (Fe) is moved in the reactor of 200 mL,
Reactor is put in 180 DEG C of baking oven, is reacted 12 hours, to be cooled to after room temperature, Jing centrifugations, redistilled water and anhydrous second
Alcohol washs 5 ~ 6 times, is dried 10 hours at 60 DEG C, and CdS/MIL-53 (Fe) visible light catalyst composite products are finally obtained.
With novel C dS/MIL-53 (Fe) visible light catalyst Jing X-ray diffraction analysis prepared by above-mentioned processing step（Figure
1b）, consisting of CdS and MIL-53 (Fe).Jing Visible Light Induced Photocatalytic rhodamine B solution testing analysis shows（Fig. 3 b）, it is to sieve
The degradation rate of red bright B solution is 78%.
CdS/MIL-53 (Fe) visible light catalyst prepared by the present invention can be widely applied to environmental pollution improvement and light is urged
Change chemical field.
Claims (1)
1. a kind of preparation method of CdS/MIL-53 (Fe) visible light catalyst, is characterized in that, with following process and step：
A. MIL-53 (Fe) is prepared
A. ferric chloride is pressed：P-phthalic acid：N,N-dimethylformamide=1：1：The ratio of 65 (mol ratios) weighs respectively trichlorine
Change ferrum, p-phthalic acid, N,N-dimethylformamide；
Described ferric chloride is ferric chloride (FeCl36H2O)；
B. the ferric chloride weighed by step a, p-phthalic acid are dissolved in DMF, are fully stirred at room temperature
Mix, ferric chloride, p-phthalic acid is fully dissolved, be configured to the N containing ferric chloride and p-phthalic acid, N- dimethyl formyls
Amine aqueous solution；
C. the N,N-dimethylformamide solution containing ferric chloride and p-phthalic acid configured by step b is moved into into 100 mL
Reactor in, reactor is put in 150 DEG C of baking oven, react 12 hours, after being cooled to room temperature, centrifugation must react
Thing；
D. will be washed with redistilled water and absolute methanol 5 ~ 6 times by step c gained reactant, place into 500 mL second distillations
The night of agitator treating one obtains washings in water；Washings are dried 10 hours at 60 DEG C, product MIL-53 (Fe) is obtained；
B. CdS is produced by cadmium acetate, thioacetamide, and CdS/MIL-53 (Fe) composite is further obtained
A. formula design requirement, CdS are pressed:MIL-53(Fe)=(1~1.5):1（Mass ratio）Calculated, taken each participation raw material
The expense of material；
B. cadmium acetate is pressed：Thioacetamide=1:The ratio of 1 (mol ratios) weighs respectively cadmium acetate and thioacetamide；
Described cadmium acetate is two water cadmium acetates；
C. polyvinylpyrrolidone is pressed：Ethylene glycol=0.2:The ratio of 100 (g/mL) weighs respectively polyvinylpyrrolidone and second two
Alcohol；
Described polyvinylpyrrolidone is PVP K-30；
D., during the MIL-53 (Fe) weighed by step a to be scattered in the 100 mL ethylene glycol measured by step c；Magnetic force at room temperature
Stirring, makes MIL-53 (Fe) fully dispersed；
E. the cadmium acetate weighed by step b is dissolved in the mixed liquor of the ethylene glycol containing MIL-53 (Fe) prepared by step d, room
The lower magnetic agitation of temperature, makes cadmium acetate fully dissolve；
F. the polyvinylpyrrolidone for weighing by the thioacetamide weighed by step b and by step c is dissolved in jointly is matched somebody with somebody by step e
In the mixed liquor of system, magnetic agitation under room temperature makes thioacetamide and polyvinylpyrrolidone fully dissolve；
G. by the ethylene glycol containing MIL-53 (Fe), cadmium acetate, thioacetamide and polyvinylpyrrolidone prepared by step f
Mixed liquor is moved in the reactor of 150 mL, and reactor is put in 180 DEG C of baking oven, is reacted 12 hours, is cooled to room
Wen Hou, centrifugation obtains reactant；
H. by the reactant redistilled water as obtained by step g and absolute ethanol washing 5 ~ 6 times, washings are obtained；By washings
It is dried at 60 DEG C 10 hours, CdS/MIL-53 (Fe) visible light catalyst composite products is finally obtained.
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