CN110302805A - A kind of single layer composite visible light catalytic material and preparation method thereof - Google Patents
A kind of single layer composite visible light catalytic material and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 29
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 21
- 239000002131 composite material Substances 0.000 title claims abstract description 21
- 239000002356 single layer Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000000243 solution Substances 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 239000011701 zinc Substances 0.000 claims description 16
- 239000000843 powder Substances 0.000 claims description 15
- 239000007787 solid Substances 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 10
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 10
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Chemical compound [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 claims description 10
- 238000002604 ultrasonography Methods 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 claims description 6
- 229920000642 polymer Polymers 0.000 claims description 6
- 239000000376 reactant Substances 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000004743 Polypropylene Substances 0.000 claims description 5
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 5
- 150000001298 alcohols Chemical class 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 239000012046 mixed solvent Substances 0.000 claims description 5
- 229920001155 polypropylene Polymers 0.000 claims description 5
- 230000001376 precipitating effect Effects 0.000 claims description 5
- 230000001681 protective effect Effects 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 5
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 5
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 5
- 239000004246 zinc acetate Substances 0.000 claims description 5
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 7
- 239000001257 hydrogen Substances 0.000 abstract description 7
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 3
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 description 9
- 230000000694 effects Effects 0.000 description 5
- 239000003643 water by type Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical group O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 239000011219 quaternary composite Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 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
-
- B01J35/39—
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/344—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy
- B01J37/346—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy of microwave energy
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/02—Processes for making hydrogen or synthesis gas
- C01B2203/0266—Processes for making hydrogen or synthesis gas containing a decomposition step
- C01B2203/0277—Processes for making hydrogen or synthesis gas containing a decomposition step containing a catalytic decomposition step
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/10—Catalysts for performing the hydrogen forming reactions
- C01B2203/1041—Composition of the catalyst
- C01B2203/1076—Copper or zinc-based catalysts
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The present invention provides a kind of single layer composite visible light catalytic material and preparation method thereof, the chemical formula of the composite visible light catalytic material is SrxZn1‑xIn2S4, wherein 0 < x < 1.Photocatalyzed Hydrogen Production with higher is active under visible light for the catalysis material.
Description
Technical field
The invention belongs to photocatalysis technology fields, and in particular to a kind of single layer quaternary SrxZn1-xIn2S4Composite visible light is urged
Change material and preparation method thereof.
Background technique
Coal burning provides electric energy for industrial development, while heating for urban life.But the waste residue that coal burning generates
Environment is seriously polluted with exhaust gas, and causes irreversible consequence, such as haze, water pollution.Rely on traditional fossil energy not
It is evitable to will cause environmental pollution, and will lead to energy crisis.During modern development in science and technology, the development of clean energy resource
Make rapid progress, wherein Hydrogen Energy is ideal clean energy resource, releases energy after hydrogen and oxygen combustion and generates water, is nothing to environment
Pollution.
The common method for producing hydrogen is electrolysis water, but the electric energy consumed is with traditional fossil energy there is still a need for being provided,
This has violated the original intention of protection environment.In recent years, using sunlight by the research of generation of hydrogen by dissociation of water and oxygen by extensive
Concern.Sunlight is inexhaustible huge energy, and water takes up an area the 70% of sphere area, therefore is by water decomposition using sunlight
Hydrogen Energy has huge scientific value.Wherein photochemical catalyst using essential.
Common photochemical catalyst is TiO2, but TiO2Ultraviolet light can only be responded, visible light cannot be utilized, caused in sunlight
Most luminous energy cannot be utilized.It has conducted extensive research in exploitation visible light catalyst work, but does not all have both at home and abroad
Reach satisfactory degree.
Pass through level structure design and many experiments, it has been found that the composite semiconductor material of sulfide composition can be by can
Light-exposed excitation makes photochemical catalyst play maximum catalytic efficiency.
Summary of the invention
The purpose of the present invention is to provide a kind of single layer quaternary SrxZn1-xIn2S4Composite visible light catalytic material and its preparation
Method.
To achieve the above object, the present invention adopts the following technical scheme:
A kind of single layer quaternary composite visible light catalytic material, chemical formula SrxZn1-xIn2S4, wherein 0 < x < 1.
A kind of single layer quaternary SrxZn1-xIn2S4The preparation method of composite visible light catalytic material, comprising the following steps:
(1) strontium nitrate x mmol (0 < x < 1), zinc acetate 1-x mmol, 2 mmol of inidum chloride, 4.5 mmol of thioacetamide are weighed
It is successively added in 250 mL three-necked flasks, 10-20 mL acetone and 10-20 mL deionized water, continual ultrasonic 0.5-1.5 is added
H, obtains uniform mixed solution, and 20 mL are added into solution using tetrahydrofuran and N ' dinethylformamide is mixed solvent
The bis- block polymer polystyrene-polypropylene acid mixed liquors of 0.5 mmol of dissolution, then 1 mmol neighbour's benzene two is dissolved in the solution
Formic acid or M-phthalic acid, 0.5 h of ultrasonic disperse；
(2) it transfers the solution into 100 mL ptfe autoclaves, it is dedicated that upper microwave is covered outside ptfe autoclave
Reaction kettle is put into microwave hydrothermal reactor by safety protective cover, and setting microwave power is 300 W, and the microwave reaction time is 1-8
H, microwave reaction temperature are 130-220 DEG C；
(3) after reaction, reactant is poured into centrifuge tube, 30 min of ultrasonic disperse, by precipitating distilled water and anhydrous second
Alcohol washs 3 times respectively, and 9000 r/min are centrifugally separating to obtain solid powder, and solid powder is transferred to equipped with 100 mL dehydrated alcohols
Beaker in, be passed through 0.1-1Mpa high pressure nitrogen in beaker bottom, be put into ultrasound 2-3 h, supersonic frequency in ultrasound reactor
It is centrifugally separating to obtain solid powder for 20~40kHz, 9000 r/min, 60-80 DEG C of 24 h of drying, pulverizes, forms one kind
Single layer quaternary SrxZn1-xIn2S4Composite visible light catalytic material.
The present invention has the advantages that the present invention makes block-shaped material using high pressure nitrogen compared with product is prepared under temperate condition
Material is stripped into stratified material, the table of surfactant (double block polymer polystyrene-polypropylene acid) effective protection material
Face form, microwave heating provide internal uniform heat source and magnetic field, are conducive to the raising of material purity.
Ternary material ZnIn2S4It is verified that having visible light catalysis activity, but also need to improve.After doped chemical Sr
Lattice defect is formd, more reaction active sites are produced, improves photocatalytic activity compared with three-way catalyst.In addition, Sr pairs
The adsorption/desorption effect of reactants and products can also influence the activity of catalyst.
The total amount of Sr and Zn is 1, and catalyst activity is related to dosage, and with the increase of Sr dosage, activity is after first increasing
Reduced variation tendency.
Detailed description of the invention
Fig. 1 is Sr0.2Zn0.8In2S4The XRD diagram of composite visible light catalytic material；
Fig. 2 is Sr0.2Zn0.8In2S4The electron microscope of composite visible light catalytic material.
Specific embodiment
To make the foregoing features and advantages of the present invention clearer and more comprehensible, special embodiment below elaborates.This hair
Bright method is conventional method in that art unless otherwise specified.
Embodiment 1
A kind of single layer quaternary Sr0.2Zn0.8In2S4The preparation method of composite visible light catalytic material, comprising the following steps:
(1) strontium nitrate 0.2mmol is weighed, 0.8 mmol of zinc acetate, 2 mmol of inidum chloride, 4.5 mmol of thioacetamide successively add
Enter into 250 mL three-necked flasks, 10 mL acetone and 10 mL deionized waters, 0.5 h of continual ultrasonic is added, obtains uniform mix
Solution is closed, 20 mL are added into solution using tetrahydrofuran and N ' 0.5 mmol that is dissolved as mixed solvent of dinethylformamide
Double block polymer polystyrene-polypropylene acid mixed liquors, then 1 mmol phthalic acid, ultrasonic disperse are dissolved in the solution
0.5 h；
(2) it transfers the solution into 100 mL ptfe autoclaves, it is dedicated that upper microwave is covered outside ptfe autoclave
Reaction kettle is put into microwave hydrothermal reactor by safety protective cover, and setting microwave power is 300 W, and the microwave reaction time is 1
H, microwave reaction temperature are 200 DEG C；
(3) after reaction, reactant is poured into centrifuge tube, 30 min of ultrasonic disperse, by precipitating distilled water and anhydrous second
Alcohol washs 3 times respectively, and 9000 r/min are centrifugally separating to obtain solid powder, and solid powder is transferred to equipped with 100 mL dehydrated alcohols
Beaker in, be passed through 1Mpa high pressure nitrogen in beaker bottom, being put into 2 h of ultrasound, supersonic frequency in ultrasound reactor is
30kHz, 9000 r/min are centrifugally separating to obtain solid powder, 60 DEG C of 24 h of drying, pulverize, form a kind of single layer quaternary
Sr0.2Zn0.8In2S4Composite visible light catalytic material.
Embodiment 2
A kind of single layer quaternary Sr0.5Zn0.5In2S4The preparation method of composite visible light catalytic material, comprising the following steps:
(1) strontium nitrate 0.5mmol is weighed, zinc acetate 0.5mmol, 2 mmol of inidum chloride, 4.5 mmol of thioacetamide successively add
Enter into 250 mL three-necked flasks, 15 mL acetone are added and it is molten to obtain uniform mixing by 15 mL deionized waters, continual ultrasonic 1h
20 mL are added into solution using tetrahydrofuran and N for liquid ' 0.5 mmol that dissolves as mixed solvent of dinethylformamide is bis- embedding
Section polymers polystyrene-polyacrylic acid mixed liquor, then 1 mmol phthalic acid is dissolved in the solution, 0.5 h of ultrasonic disperse；
(2) it transfers the solution into 100 mL ptfe autoclaves, it is dedicated that upper microwave is covered outside ptfe autoclave
Reaction kettle is put into microwave hydrothermal reactor by safety protective cover, and setting microwave power is 300 W, and the microwave reaction time is 5h,
Microwave reaction temperature is 130 DEG C；
(3) after reaction, reactant is poured into centrifuge tube, 30 min of ultrasonic disperse, by precipitating distilled water and anhydrous second
Alcohol washs 3 times respectively, and 9000 r/min are centrifugally separating to obtain solid powder, and solid powder is transferred to equipped with 100 mL dehydrated alcohols
Beaker in, be passed through 0.5Mpa high pressure nitrogen in beaker bottom, being put into ultrasound 2h, supersonic frequency in ultrasound reactor is
40kHz, 9000 r/min are centrifugally separating to obtain solid powder, 70 DEG C of 24 h of drying, pulverize, form a kind of single layer quaternary
Sr0.5Zn0.5In2S4Composite visible light catalytic material.
Embodiment 3
A kind of single layer quaternary Sr0.9Zn0.1In2S4The preparation method of composite visible light catalytic material, comprising the following steps:
(1) strontium nitrate 0.9mmol is weighed, 0.1 mmol of zinc acetate, 2 mmol of inidum chloride, 4.5 mmol of thioacetamide successively add
Enter into 250 mL three-necked flasks, 20 mL acetone and 20 mL deionized waters, 1.5 h of continual ultrasonic is added, obtains uniform mix
Solution is closed, 20 mL are added into solution using tetrahydrofuran and N ' 0.5 mmol that is dissolved as mixed solvent of dinethylformamide
Double block polymer polystyrene-polypropylene acid mixed liquors, then 1 mmol M-phthalic acid, ultrasonic disperse are dissolved in the solution
0.5 h；
(2) it transfers the solution into 100 mL ptfe autoclaves, it is dedicated that upper microwave is covered outside ptfe autoclave
Reaction kettle is put into microwave hydrothermal reactor by safety protective cover, and setting microwave power is 300 W, and the microwave reaction time is 8
H, microwave reaction temperature are 220 DEG C；
(3) after reaction, reactant is poured into centrifuge tube, 30 min of ultrasonic disperse, by precipitating distilled water and anhydrous second
Alcohol washs 3 times respectively, and 9000 r/min are centrifugally separating to obtain solid powder, and solid powder is transferred to equipped with 100 mL dehydrated alcohols
Beaker in, be passed through 0.1Mpa high pressure nitrogen in beaker bottom, being put into 3 h of ultrasound, supersonic frequency in ultrasound reactor is
20kHz, 9000 r/min are centrifugally separating to obtain solid powder, 80 DEG C of 24 h of drying, pulverize, form a kind of single layer quaternary
Sr0.9Zn0.1In2S4Composite visible light catalytic material.
In fixed bed reactors, under the irradiation of 300W xenon lamp, 90 ml deionized waters and 10 ml methanols form mixed liquor,
The catalyst in 0.1g embodiment 1 is added, magnetic agitation is reacted 8 hours and stopped.Through gas chromatographic detection, hydrogen output is
(139 umol/g/h)。
Fig. 1 is the XRD diagram of catalyst, and the position at the peak Cong Tuzhong, which can be seen that, generates target product, and peak type is sharp, explanation
Complete crystal form.Fig. 2 is the SEM figure of sample, and as can be seen from the figure the microscopic appearance of sample, sample are sheet-like morphology.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, is all covered by the present invention.
Claims (2)
1. a kind of single layer composite visible light catalytic material, which is characterized in that the chemistry of the single layer composite visible light catalytic material
Formula is SrxZn1-xIn2S4, wherein 0 < x < 1.
2. the preparation method of single layer composite visible light catalytic material according to claim 1, which is characterized in that including following
Step:
(1) strontium nitrate x mmol is weighed, zinc acetate 1-x mmol, 2 mmol of inidum chloride, 4.5 mmol of thioacetamide successively add
Enter into 250 mL three-necked flasks, 10-20 mL acetone is added and 10-20 mL deionized water, continual ultrasonic 0.5-1.5 h are obtained
To uniform mixed solution, 20 mL are added into solution using tetrahydrofuran and N ' dinethylformamide as mixed solvent dissolve
The bis- block polymer polystyrene-polypropylene acid mixed liquors of 0.5 mmol, then dissolve 1 mmol phthalic acid in the solution
Or M-phthalic acid, 0.5 h of ultrasonic disperse；
(2) it transfers the solution into 100 mL ptfe autoclaves, it is dedicated that upper microwave is covered outside ptfe autoclave
Reaction kettle is put into microwave hydrothermal reactor by safety protective cover, and setting microwave power is 300 W, and the microwave reaction time is 1-8
H, microwave reaction temperature are 130-220 DEG C；
(3) after reaction, reactant is poured into centrifuge tube, 30 min of ultrasonic disperse, by precipitating distilled water and anhydrous second
Alcohol washs 3 times respectively, and 9000 r/min are centrifugally separating to obtain solid powder, and solid powder is transferred to equipped with 100 mL dehydrated alcohols
Beaker in, be passed through 0.1-1Mpa high pressure nitrogen in beaker bottom, be put into ultrasound 2-3 h, supersonic frequency in ultrasound reactor
It is centrifugally separating to obtain solid powder for 20~40kHz, 9000 r/min, 60-80 DEG C of 24 h of drying, pulverizes, obtains single layer
SrxZn1-xIn2S4Composite visible light catalytic material, wherein 0 < x < 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910642087.5A CN110302805B (en) | 2019-07-16 | 2019-07-16 | Single-layer composite visible light catalytic material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910642087.5A CN110302805B (en) | 2019-07-16 | 2019-07-16 | Single-layer composite visible light catalytic material and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110302805A true CN110302805A (en) | 2019-10-08 |
| CN110302805B CN110302805B (en) | 2022-06-07 |
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