CN108452813A - A kind of MoS2/SrFe12O19The preparation method of composite magnetic photochemical catalyst - Google Patents
A kind of MoS2/SrFe12O19The preparation method of composite magnetic photochemical catalyst Download PDFInfo
- Publication number
- CN108452813A CN108452813A CN201810243281.1A CN201810243281A CN108452813A CN 108452813 A CN108452813 A CN 108452813A CN 201810243281 A CN201810243281 A CN 201810243281A CN 108452813 A CN108452813 A CN 108452813A
- Authority
- CN
- China
- Prior art keywords
- srfe
- mos
- photochemical catalyst
- preparation
- composite magnetic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 52
- 239000003054 catalyst Substances 0.000 title claims abstract description 37
- 239000002131 composite material Substances 0.000 title claims abstract description 37
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 229910052961 molybdenite Inorganic materials 0.000 title claims abstract description 23
- 229910002402 SrFe12O19 Inorganic materials 0.000 claims abstract description 67
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 6
- 238000011084 recovery Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 21
- 239000003153 chemical reaction reagent Substances 0.000 claims description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 239000000725 suspension Substances 0.000 claims description 9
- 239000012065 filter cake Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000013019 agitation Methods 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- 239000003643 water by type Substances 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 230000001699 photocatalysis Effects 0.000 claims description 5
- ZNNZYHKDIALBAK-UHFFFAOYSA-M potassium thiocyanate Chemical compound [K+].[S-]C#N ZNNZYHKDIALBAK-UHFFFAOYSA-M 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000004090 dissolution Methods 0.000 claims description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 3
- 101100496858 Mus musculus Colec12 gene Proteins 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 13
- 230000015556 catabolic process Effects 0.000 abstract description 9
- 238000006731 degradation reaction Methods 0.000 abstract description 9
- 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 7
- 229940043267 rhodamine b Drugs 0.000 abstract description 6
- 230000008901 benefit Effects 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 4
- 238000012545 processing Methods 0.000 abstract description 3
- 229910052724 xenon Inorganic materials 0.000 abstract description 3
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 abstract description 3
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 239000010919 dye waste Substances 0.000 abstract description 2
- 230000008569 process Effects 0.000 abstract description 2
- 230000001681 protective effect Effects 0.000 abstract description 2
- 239000000758 substrate Substances 0.000 abstract 1
- 238000010521 absorption reaction Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- 238000004064 recycling Methods 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 6
- 229910052712 strontium Inorganic materials 0.000 description 6
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 6
- 238000012512 characterization method Methods 0.000 description 5
- 230000005415 magnetization Effects 0.000 description 5
- 239000011941 photocatalyst Substances 0.000 description 5
- 238000011160 research Methods 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 229910000859 α-Fe Inorganic materials 0.000 description 4
- 230000000593 degrading effect Effects 0.000 description 3
- 239000000975 dye Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000013066 combination product Substances 0.000 description 2
- 229940127555 combination product Drugs 0.000 description 2
- 238000002242 deionisation method Methods 0.000 description 2
- 238000004880 explosion Methods 0.000 description 2
- 238000009830 intercalation Methods 0.000 description 2
- 230000002687 intercalation Effects 0.000 description 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000002060 nanoflake Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000005493 condensed matter Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 229910001410 inorganic ion Inorganic materials 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000010815 organic waste Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- OXNIZHLAWKMVMX-UHFFFAOYSA-N picric acid Chemical compound OC1=C([N+]([O-])=O)C=C([N+]([O-])=O)C=C1[N+]([O-])=O OXNIZHLAWKMVMX-UHFFFAOYSA-N 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002459 sustained effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 238000003911 water pollution Methods 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
-
- 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
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
- B01J27/0515—Molybdenum with iron group metals or platinum group metals
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Toxicology (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Catalysts (AREA)
Abstract
A kind of MoS2/SrFe12O19The preparation method of composite magnetic photochemical catalyst belongs to nano inorganic catalysis material field.The present invention uses hydro-thermal method, is first prepared for magnetic substrate SrFe12O19, then it is prepared for MoS2/SrFe12O19Composite magnetic photochemical catalyst.MoS2/SrFe12O19Composite magnetic photochemical catalyst crystallinity is good, has preferable magnetic property.Under the xenon lamp irradiation of simulated solar irradiation, composite magnetic photochemical catalyst prepared by 50mg, the rhodamine B solution of degradation 100mL a concentration of 10mg/L, the degradation rate in 90min is 95.2%, and the average recovery rate of catalyst is 67%.Preparation process of the present invention is easy, easily controllable, and production efficiency is high and at low cost, environmentally protective using process, and the processing to industrializing organic dye waste water has advantage outstanding.
Description
Technical field
The present invention relates to a kind of MoS2/SrFe12O19The preparation method of composite magnetic photochemical catalyst belongs to inorganic environment-friendly catalysis
Field of material technology.
Background technology
The photocatalysis field of nano material is as a kind of emerging research field covering multi-crossed disciplines, it has also become solves light
The hot research direction of water pollution, industrial wastewater treatment and clear energy sources production technology.Wherein, with molybdenum disulfide (MoS2) it is generation
The transient metal sulfide of table relies on its superior physicochemical property, is widely applied to metal lubrication, two pole of lithium battery photoelectricity
Pipe, energy storage and conversion etc..Meanwhile MoS2Layer structure and semiconductor property with similar graphite, have ratio
The characteristics such as surface area is big, adsorption capacity is strong, the MoS of different crystal structure2Energy gap is smaller, only 1.29eV-1.9eV it
Between, therefore valence-band electrons can occur transition and enter conduction band under visible light illumination, and hole is left, to generate electron-hole
It is right, there is the preferable potential quality as photochemical catalyst.Especially when grain size scale is down to nanoscale, MoS2Reactivity improves
While, chemical stability weakens there is no apparent, shows that it has as semi-conducting material in optical electro-chemistry reaction
Excellent corrosion resistance, this is that many semi-conducting materials with compared with low energy gap are short of.Therefore, MoS2It has become novel
The hot research object of photochemical catalyst exploitation.
Current pertinent literature is reported, for MoS2Modification and its compound achievement in research it is more, such as
“Enhancedphotocatalytic activity of ZnS nanoparticles loaded with
MoS2nanoflakes by self-assemblyapproach”(Physica B:Condensed Matter,2016,502:
103-112) one literary (documents 1), this article use hydro-thermal method, first prepare ZnS nano particles and MoS respectively2Nano flake,
The two is dissolved in ethyl alcohol again and being mixed, after mixed solution again high temperature and pressure hydro-thermal reaction, generates two compounds.It should
Main problem existing for method is：(1) preparation process needs to undergo three steps altogether, can just obtain combination product, manufacturing cycle
Longer, of high cost, the consumed energy is larger, is not suitable for promoting；(2) only suitable treatment low-concentration organic waste water, photochemical catalyst are being thrown
High-volume under conditions of 0.5g/L, for the rhodamine B aqueous solution of a concentration of 5mg/L of the 100mL that degrades, degradation rate is after 90min
90% or so；(3) there is recycling hardly possible, easily cause secondary pollution problems in composite catalyst.
Based on this, it is contemplated that during photocatalytic degradation organic wastewater, especially processing waste water is usually deposited on a large scale
In the difficult problem of catalyst recycling.Photochemical catalyst recycling in order to prevent is not thorough and generates secondary pollution and reduce use cost,
Photochemical catalyst is assigned into magnetic, is very necessary convenient for separation and recovery.According to existing pertinent literature, the research of magnetic photocatalyst
Work is in developing stage, and the selection of magnetisable material is mainly the Fe of soft magnetism3O4For magnetic matrix, such as Chinese invention patent
CN201610144309.7 discloses a kind of " stratiform MoS2-Fe3O4Nanocomposite and preparation method thereof " (documents 2),
Main preparation methods are combined with explosion high temperature impact by sol-gel method, by MoS2Powder first carries out layering reaction, then adds
Enter oxidant and carry out intercalation, by the intercalation MoS of generation2It is mixed with colloidal sol, using explosion so that Fe3O4Occur reduction and
MoS2Stripping, to obtain magnetic layered combination product.This method the problem is that：(1) preparation condition is harsh, complicated, system
It needs to carry out explosive reaction during standby, used burster (picric acid) is dangerous larger, for large-scale industrialization
It produces and is not suitable for；(2) composite magnetic saturation magnetization made from is relatively low, coercivity is smaller, the effect of externally-applied magnetic field
It easily loses magnetism after lower magnetization, recovering effect is bad, does not provide the data of the rate of recovery in text.Strontium ferrite (SrFe12O19) conduct
A kind of retentive material is a kind of n-type semiconductor photochemical catalyst of visible CD-ROM drive, and energy gap is smaller (1.8eV), with above-mentioned biography
The metal soft magnetic material Fe of system3O4It compares, coercivity is higher, anti-demagnetization capability is stronger, it is most important that the strontium reserves in China fill
Foot, can be widely used.For this purpose, the present invention is with SrFe12O19For magnetic matrix, composite magnetic photochemical catalyst is prepared, is carried with this
High MoS2Photocatalysis effect and assign magnetic property, convenient for detaching and recycling.
Invention content
The technical problem to be solved by the present invention is to provide a kind of MoS2/SrFe12O19The preparation side of composite magnetic photochemical catalyst
Method, core is to synthesize the composite magnetic photochemical catalyst that magnetic performance is excellent and stablizes, in raising MoS2Photocatalytic activity
Meanwhile effectively solving the problems, such as difficult recycling and its secondary pollution caused by environment.Preparation process of the present invention is easy, is easy to control
System, production efficiency is high and at low cost, and the processing to industrializing organic dye waste water has advantage outstanding, while also expanding
MoS2And its utilization of composite material photocatalyst.
MoS of the present invention2/SrFe12O19The preparation method of composite magnetic photochemical catalyst is as follows：
(1)SrFe12O19Preparation
0.7465g SrCl are weighed respectively2·6H2O and 6.0545g FeCl3·6H2O reagents are super with 38mL deionized waters
Sound dissolves to obtain mixed solution A；8.736g NaOH reagents are weighed, solution B is obtained with 20mL deionized water ultrasonic dissolutions；In perseverance
Under warm 20 DEG C of water-baths and magnetic agitation, solution B is slowly added drop-wise in mixed solution A, and continues to stir 15min, waits for solution
It is sufficiently mixed to obtain SrFe12O19Presoma C；Presoma C is poured into 100mL water heating kettles, reacts at 200 DEG C and takes out for 24 hours, from
It is so cooled to room temperature, filters, and after being washed with deionized to filtrate and being in neutrality, filter cake is placed in 80 DEG C of baking ovens dry 12h,
Grinding is taken out, SrFe is obtained12O19。
(2)MoS2/SrFe12O19Preparation
0.4319g MoO are weighed respectively3It with 0.8746g KSCN reagents, is added in 60mL deionized waters, ultrasonic 15min
And mechanical agitation 30min makes it be sufficiently mixed to obtain solution A；SrFe is generated according to theory12O19Quality percentage in the composite
Number 5wt%~15wt%, weighs the SrFe prepared12O19Powder is added in solution A, and continued mechanical stirs 1h, obtains
Suspension B is fitted into the water heating kettle of 100mL by suspension B, is reacted at 200 DEG C and is taken out for 24 hours, is cooled to room temperature, is filtered, uses
Alternately filter cake for several times, is placed in 80 DEG C of baking ovens dry 12h by washing for deionized water and absolute ethyl alcohol, to get to MoS after grinding2/
SrFe12O19。
The present invention uses above-mentioned technical proposal, mainly has the following effects：
(1) MoS prepared by the method for the present invention2/SrFe12O19Composite magnetic photochemical catalyst has higher photocatalytic activity,
Under the irradiation of simulated solar irradiation xenon lamp, with a concentration of 10mg/ of optimal composite magnetic photocatalyst for degrading 100mL of 50mg preparations
The rhodamine B solution of L, degradation rate reaches 95.2% (documents 1, the present invention is for target dye, rhodamine of degrading when 90min
The concentration of B and the degradation rate of synchronization are above the part mentioned in file 1), illustrate prepared by the method for the present invention
MoS2/SrFe12O19Composite magnetic photochemical catalyst has certain degradation advantage for high concentration dyestuff.
(2) a kind of MoS prepared by the method for the present invention2/SrFe12O19Composite magnetic photochemical catalyst is more in the case where adding magnetic fields outside
Secondary recycling, average recovery rate 67%, wherein MoS2/SrFe12O19The saturation magnetization (Ms) of (10wt%) is 10.14emu/
G, coercivity (Hci) are 1407.7Oe (magnetic property is better than documents 2).
(3) present invention uses hydro-thermal method, and easy to operate, safety and environmental protection, production efficiency is high, is suitble to promote.
Description of the drawings
Fig. 1 is SrFe12O19、MoS2/SrFe12O19And MoS2X ray diffracting spectrum；
Fig. 2 is MoS2/SrFe12O19Field emission scanning electron microscope SEM figure；
Fig. 3 is MoS2、MoS2/SrFe12O19And SrFe12O19Infrared spectrogram；
Fig. 4 is SrFe12O19And MoS2/SrFe12O19Hysteresis loop figure.
Specific implementation mode
With reference to embodiment, it further illustrates the present invention.
Embodiment 1
A kind of MoS2/SrFe12O19The preparation method of composite magnetic photochemical catalyst, is as follows：
(1)SrFe12O19Preparation
0.7465g SrCl are weighed respectively2·6H2O and 6.0545g FeCl3·6H2O reagents are super with 38mL deionized waters
Sound dissolves to obtain mixed solution A；8.736g NaOH reagents are weighed, solution B is obtained with 20mL deionized water ultrasonic dissolutions；In perseverance
Under the action of warm 20 DEG C of water-baths and magnetic agitation, solution B is slowly added drop-wise in mixed solution A, and continues stirring 15min and waits for
Solution is sufficiently mixed to obtain SrFe12O19Presoma C；Presoma C is poured into 100mL water heating kettles, reacts at 200 DEG C and takes for 24 hours
Go out, cooled to room temperature, filter, and after being washed with deionized to filtrate and being in neutrality, filter cake is placed in 80 DEG C of baking ovens and is done
Dry 12h takes out grinding, obtains SrFe12O19。
(2)MoS2/SrFe12O19Preparation
0.4319g MoO are weighed respectively3It with 0.8746g KSCN reagents, is added in 60mL deionized waters, ultrasonic 15min
And mechanical agitation 30min makes it be sufficiently mixed to obtain solution A；SrFe is generated according to theory12O19Quality percentage in the composite
Number 5wt%, weighs the SrFe prepared12O19Powder is added in solution A, and continued mechanical stirs 1h, obtains suspension B,
Suspension B is fitted into the water heating kettle of 100mL, reacts at 200 DEG C and takes out for 24 hours, room temperature is cooled to, filters, use deionized water
Alternately filter cake for several times, is placed in 80 DEG C of baking ovens dry 12h by washing with absolute ethyl alcohol, to get to MoS after grinding2/SrFe12O19。
Embodiment 2
A kind of MoS2/SrFe12O19The preparation method of composite magnetic photochemical catalyst, is as follows：
(1) with (1) the step of embodiment 1.
(2)MoS2/SrFe12O19Preparation
0.4319g MoO are weighed respectively3It with 0.8746g KSCN reagents, is added in 60mL deionized waters, ultrasonic 15min
And mechanical agitation 30min makes it be sufficiently mixed to obtain solution A；SrFe is generated according to theory12O19Quality percentage in the composite
Number 10wt%, weighs the SrFe prepared12O19Powder is added in solution A, and continued mechanical stirs 1h, obtains suspension
Suspension B is fitted into the water heating kettle of 100mL by B, is reacted at 200 DEG C and is taken out for 24 hours, is cooled to room temperature, is filtered, uses deionization
Alternately filter cake for several times, is placed in 80 DEG C of baking ovens dry 12h by washing for water and absolute ethyl alcohol, to get to MoS after grinding2/
SrFe12O19。
Embodiment 3
A kind of MoS2/SrFe12O19The preparation method of composite magnetic photochemical catalyst, is as follows：
(1) with (1) the step of embodiment 1.
(2)MoS2/SrFe12O19Preparation
0.4319g MoO are weighed respectively3It with 0.8746g KSCN reagents, is added in 60mL deionized waters, ultrasonic 15min
And mechanical agitation 30min makes it be sufficiently mixed to obtain solution A；SrFe is generated according to theory12O19Quality percentage in the composite
Number 15wt%, weighs the SrFe prepared12O19Powder is added in solution A, and continued mechanical stirs 1h, obtains suspension
Suspension B is fitted into the water heating kettle of 100mL by B, is reacted at 200 DEG C and is taken out for 24 hours, is cooled to room temperature, is filtered, uses deionization
Alternately filter cake for several times, is placed in 80 DEG C of baking ovens dry 12h by washing for water and absolute ethyl alcohol, to get to MoS after grinding2/
SrFe12O19。
Experimental result
MoS prepared by embodiment 22/SrFe12O19Catalytic degradation activity is best.In order to facilitate comparison, it is prepared for MoS2Sample
Product.MoS2Preparation method is to be added without SrFe in 2 step of embodiment (2)12O19。
SrFe prepared by the present invention12O19、MoS2/SrFe12O19And MoS2XRD characterization it is as shown in fig. 1, wherein (a)
For SrFe12O19X-ray diffractogram, 2-Theta be located at 23.19 °, 30.39 °, 31.02 °, 32.36 °, 34.22 °, 37.18 °,
Characteristic peak at 40.43 °, 42.53 °, 55.18 °, 55.82 °, 57.46 ° and 63.12 °, is respectively belonging to M-type strontium ferrite
SrFe12O19(006) of (JCPDS card No.33-1340), (110), (008), (107), (114), (203), (205),
(206), (217), (0014), (218) and (220) crystal face；(c) is MoS in figure2X-ray diffractogram, 2-Theta is located at
Diffraction maximum at 14.37 °, 29.02 °, 32.67 ° and 58.33 ° corresponds to 2H types molybdenum sulfide MoS in standard card respectively2(JCPDS
Card No.37-1492) (002), (004), (100) and (110) crystal face；By comparison, (b) is to use present invention side in figure
MoS prepared by method2/SrFe12O19Composite magnetic photochemical catalyst, the characteristic diffraction peak of X-ray and above-mentioned SrFe12O19With
MoS2Characteristic peak correspond, each peak shape is all more apparent, sharp and symmetrical, illustrates that product crystallization is complete, crystals
Both there is SrFe in spectrogram in particle queueing discipline12O19Diffraction maximum, also have MoS2Diffraction maximum, illustrate MoS2/SrFe12O19It is multiple
It closes magnetic photocatalytic to be made of hexagonal phase crystallographic system 2H types molybdenum sulfide and M-type strontium ferrite, there is its relevant characteristic, knot
Structure is stablized.
The characterization result of scanning electron microscope sem is as shown in Fig. 2, be from left to right followed successively by MoS2、SrFe12O19And MoS2/
SrFe12O19.As can be seen that the MoS prepared using hydro-thermal method2, the constituencies SEM pattern is bouquet tufted, it is by ultra-thin wadding
The bouquet that synusia is formed stacks one by one, in figure under the conditions of amplification factor is 1 μm visual, it can be clearly seen that thin layer；Figure
Middle SrFe12O19SEM patterns be regular hexagon sheet, per lamellar spacing be about 0.196-0.332 μm, pattern is complete, without miscellaneous
Matter generates, and is consistent with the ferritic shape characteristic of M-type strontium corresponding to above-mentioned XRD characterization result；MoS in figure2/SrFe12O19It is multiple
The constituencies the SEM pattern for closing magnetic photocatalyst is shown, in MoS2It is mingled with SrFe in bouquet cluster12O19Regular hexagon lamella, from
It can be seen that in figure, composite sample meets the characters and appearances of molybdenum disulfide and strontium ferrite simultaneously, it was demonstrated that according to the method for the present invention
MoS has successfully been prepared2/SrFe12O19Composite magnetic photochemical catalyst, and product shape characteristic is apparent.
MoS prepared by the method for the present invention2、MoS2/SrFe12O19And SrFe12O19Infrared spectrum characterization result such as Fig. 3
It is shown, in characteristic area, wave number 3447.4cm-1、1639.5cm-1The relatively strong absworption peak at place is the compound of sample surface
The hydroxyl O-H stretching vibrations and bending vibration of oxide adsorbent water are formed by absorption vibration peak；In 2913.7cm-1The suction of left and right
It receives caused by the stretching vibration that peak is c h bond；And 2347cm-1The Weak Absorption peak of left and right is speculated as CO2Antisymmetry is stretched institute
It causes；Wherein, it can be seen that by the characteristic absorption peak shown by fingerprint region, MoS2/SrFe12O19Composite magnetic photochemical catalyst exists
435.5cm-1、548.4cm-1And 586.8cm-1The absorption peak at place belongs to SrFe12O19Characteristic absorption peak；In 418.9cm-1's
Absorption peak is Mo-S keys, it and 457.2cm-1The absorption peak at place belongs to MoS2, other miscellaneous peaks, above-mentioned table are not shown in spectrogram
Sign result is consistent with document, it was demonstrated that MoS of the present invention2/SrFe12O19The preparation method of composite magnetic photochemical catalyst is effective.
It has been shown that, a kind of MoS prepared by the method for the present invention are tested in conjunction with the photocatalysis that above-mentioned characterization result carries out2/SrFe12O19
Composite magnetic photochemical catalyst, SrFe12O19Mass percent be 10wt% when, under the irradiation of simulated solar irradiation xenon lamp, use
The rhodamine B solution of a concentration of 10mg/L of composite magnetic photocatalyst for degrading 100mL prepared by 50mg, 90min is to rhodamine B
Degradation rate reaches 95.2%, illustrates the MoS prepared using the present invention2/SrFe12O19Composite magnetic photochemical catalyst has higher light
Catalytic activity has stronger utilization conversion and absorption to simulated solar irradiation, can accelerate to generate electron-hole pair so that
Reaction of formation activity preferably OH free radicals are reacted in hole with water, and dyestuff is degraded to inorganic ions and organic molecule, and
Repeatedly after recycling, 70% or more is maintained to the degradation rate of rhodamine B.
SrFe12O19And MoS2/SrFe12O19Magnetic parameter test results are shown in figure 4, SrFe12O19Saturated magnetization
Intensity (Ms) is 58.08emu/g, coercivity (Hci) is 793.4Oe；MoS2/SrFe12O19Saturation magnetization is 10.14emu/
G, coercivity is 1407.7Oe；The said goods prepared in the process of the present invention possess stronger magnetic performance advantage, especially institute
The compound sample prepared, coercivity are obviously improved, and are conducive to the recycling of photochemical catalyst, environmentally protective, are effectively solved
After catalyst use caused by environment secondary pollution problem.
Embodiment above describes the preparation method of the present invention, main features and advantages.The present invention is not by above-described embodiment
Limitation, under the range for not departing from the principle of the invention, method, for the present invention by sustained improvement, these each fall within protection of the present invention
In the range of.
Claims (2)
1. a kind of MoS2/SrFe12O19The preparation method of composite magnetic photochemical catalyst, feature include the following steps：
(1)SrFe12O19Preparation
0.7465g SrCl are weighed respectively2·6H2O and 6.0545g FeCl3·6H2O reagents, with 38mL deionized water ultrasonic dissolutions
Obtain mixed solution A；8.736g NaOH reagents are weighed, solution B is obtained with 20mL deionized water ultrasonic dissolutions；In 20 DEG C of constant temperature
Under water-bath and magnetic agitation, solution B is slowly added drop-wise in mixed solution A, and continues to stir 15min, waits for that solution is fully mixed
Conjunction obtains SrFe12O19Presoma C；Presoma C is poured into 100mL water heating kettles, reacts at 200 DEG C and takes out for 24 hours, natural cooling
It to room temperature, filters, and after being washed with deionized to filtrate and being in neutrality, filter cake is placed in 80 DEG C of baking ovens dry 12h, taking-up is ground
Mill, obtains SrFe12O19。
(2)MoS2/SrFe12O19Preparation
0.4319g MoO are weighed respectively3It with 0.8746g KSCN reagents, is added in 60mL deionized waters, ultrasonic 15min and machine
Tool stirring 30min makes it be sufficiently mixed to obtain solution A；SrFe is generated according to theory12O19Mass percent in the composite
5wt%~15wt% weighs the SrFe prepared12O19Powder is added in solution A, and continued mechanical stirs 1h, is hanged
Suspension B is fitted into the water heating kettle of 100mL by turbid B, is reacted at 200 DEG C and is taken out for 24 hours, is cooled to room temperature, is filtered, spends
Alternately filter cake for several times, is placed in 80 DEG C of baking ovens dry 12h by washing for ionized water and absolute ethyl alcohol, to get to MoS after grinding2/
SrFe12O19。
2. MoS according to claim 12/SrFe12O19The preparation method of composite magnetic photochemical catalyst, it is characterised in that with
Prepared by hydro-thermal method, the photocatalytic activity of composite magnetic photochemical catalyst is high, and can be by Recovery of magnetic medium.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810243281.1A CN108452813B (en) | 2018-03-23 | 2018-03-23 | MoS2/SrFe12O19Preparation method of composite magnetic photocatalyst |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810243281.1A CN108452813B (en) | 2018-03-23 | 2018-03-23 | MoS2/SrFe12O19Preparation method of composite magnetic photocatalyst |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108452813A true CN108452813A (en) | 2018-08-28 |
| CN108452813B CN108452813B (en) | 2021-03-23 |
Family
ID=63237111
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810243281.1A Expired - Fee Related CN108452813B (en) | 2018-03-23 | 2018-03-23 | MoS2/SrFe12O19Preparation method of composite magnetic photocatalyst |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108452813B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110090652A (en) * | 2019-05-07 | 2019-08-06 | 重庆大学 | A method of it preparing chlorine four and aoxidizes three bismuths/strontium ferrite composite magnetic catalysis material |
| CN111974418A (en) * | 2020-07-13 | 2020-11-24 | 重庆大学 | Preparation of ternary composite magnetic photocatalytic material MoS2/WO3/SrFe12O19Method (2) |
| CN111974407A (en) * | 2020-07-13 | 2020-11-24 | 重庆大学 | Method for preparing magnetic tungsten trioxide composite photocatalyst |
| CN114950463A (en) * | 2022-07-01 | 2022-08-30 | 重庆大学 | Novel magnetic composite photocatalyst MoO 3 /SrFe 12 O 19 Preparation method of (1) |
| CN115041182A (en) * | 2022-07-12 | 2022-09-13 | 重庆大学 | Magnetic ternary composite photocatalyst In-MoO 3 /SrFe 12 O 19 Preparation method of (1) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006075684A (en) * | 2004-09-07 | 2006-03-23 | Noritake Co Ltd | Inorganic porous body for carrying photocatalyst |
| CN103028352A (en) * | 2012-12-10 | 2013-04-10 | 江苏大学 | Preparation method for synthesizing MoS2/Fe3O4 nano composite material |
| CN103480384A (en) * | 2013-09-18 | 2014-01-01 | 重庆大学 | Preparation method for bismuth vanadate composite photocatalyst loaded with strontium ferrite |
| CN106799246A (en) * | 2017-02-26 | 2017-06-06 | 河南师范大学 | A kind of magnetic MoS2@Fe3O4Composite visible light catalyst and its preparation method and application |
| CN107349940A (en) * | 2017-08-11 | 2017-11-17 | 中国科学院东北地理与农业生态研究所 | A kind of preparation method and applications of the cobalt ferrite photochemical catalyst of Z-type magnetic nanometer composite material molybdenum disulfide/tetra- oxygen two |
-
2018
- 2018-03-23 CN CN201810243281.1A patent/CN108452813B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006075684A (en) * | 2004-09-07 | 2006-03-23 | Noritake Co Ltd | Inorganic porous body for carrying photocatalyst |
| CN103028352A (en) * | 2012-12-10 | 2013-04-10 | 江苏大学 | Preparation method for synthesizing MoS2/Fe3O4 nano composite material |
| CN103480384A (en) * | 2013-09-18 | 2014-01-01 | 重庆大学 | Preparation method for bismuth vanadate composite photocatalyst loaded with strontium ferrite |
| CN106799246A (en) * | 2017-02-26 | 2017-06-06 | 河南师范大学 | A kind of magnetic MoS2@Fe3O4Composite visible light catalyst and its preparation method and application |
| CN107349940A (en) * | 2017-08-11 | 2017-11-17 | 中国科学院东北地理与农业生态研究所 | A kind of preparation method and applications of the cobalt ferrite photochemical catalyst of Z-type magnetic nanometer composite material molybdenum disulfide/tetra- oxygen two |
Non-Patent Citations (1)
| Title |
|---|
| 谢太平 等: "锶磁性光催化剂的制备和表征", 《功能材料》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110090652A (en) * | 2019-05-07 | 2019-08-06 | 重庆大学 | A method of it preparing chlorine four and aoxidizes three bismuths/strontium ferrite composite magnetic catalysis material |
| CN111974418A (en) * | 2020-07-13 | 2020-11-24 | 重庆大学 | Preparation of ternary composite magnetic photocatalytic material MoS2/WO3/SrFe12O19Method (2) |
| CN111974407A (en) * | 2020-07-13 | 2020-11-24 | 重庆大学 | Method for preparing magnetic tungsten trioxide composite photocatalyst |
| CN114950463A (en) * | 2022-07-01 | 2022-08-30 | 重庆大学 | Novel magnetic composite photocatalyst MoO 3 /SrFe 12 O 19 Preparation method of (1) |
| CN114950463B (en) * | 2022-07-01 | 2023-09-08 | 重庆大学 | Novel magnetic composite photocatalyst MoO 3 /SrFe 12 O 19 Is prepared by the preparation method of (2) |
| CN115041182A (en) * | 2022-07-12 | 2022-09-13 | 重庆大学 | Magnetic ternary composite photocatalyst In-MoO 3 /SrFe 12 O 19 Preparation method of (1) |
| CN115041182B (en) * | 2022-07-12 | 2023-06-09 | 重庆大学 | Magnetic ternary composite photocatalyst In-MoO 3 /SrFe 12 O 19 Is prepared by the preparation method of (2) |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108452813B (en) | 2021-03-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108452813A (en) | A kind of MoS2/SrFe12O19The preparation method of composite magnetic photochemical catalyst | |
| CN106984261A (en) | A kind of CoFe2O4/ N/C hollow nano-spheres and its preparation and application | |
| Xu et al. | Preparation and photocatalytic property of spindle-like MIL-88B (Fe) nanoparticles | |
| CN108704611A (en) | It is a kind of magnetism manganese iron axinite load mesoporous fiber element charcoal composite material and preparation method with application | |
| CN107837816B (en) | Fe2O3/g-C3N4Composite system, preparation method and application | |
| CN109647445B (en) | MoS2Nanosheet-coated KNbO3Preparation method of nanowire piezoelectric/photocatalytic material | |
| CN102942165A (en) | Graphene and ferrum diselenide composite material and method for preparing same | |
| CN108579661A (en) | A kind of doped modified lithium ion sieve and preparation method thereof, application | |
| CN104577131A (en) | Preparation method of graphite-TiO2-B composite material | |
| CN107240508A (en) | A kind of preparation method of graphene/ferrite nano combination electrode material | |
| CN106115798B (en) | A kind of MnCo2O4Hexagonal nanometer rods and method for preparing Nano cube | |
| CN107890861B (en) | Preparation method of titanium dioxide lamella/graphene composite film with {001} crystal face | |
| CN109665525A (en) | A kind of preparation method of " dumbbell shape " iron nitrogen codope porous carbon | |
| CN103447024B (en) | The preparation method of a kind of bismuthino strontium magnetic photocatalyst and bismuthino strontium magnetic photocatalyst thereof | |
| Jiang et al. | Magnetic recyclable ZnO/SrFe12O19 photocatalyst for effective photodegradation of rhodamine B under simulated sunlight | |
| CN103111300B (en) | Method for preparing TiO2/ni-zn ferrite/carbon (C) magnetic photocatalyst | |
| CN111974407A (en) | Method for preparing magnetic tungsten trioxide composite photocatalyst | |
| CN109675521B (en) | Graphene oxide-gadolinium hydroxide composite material, preparation method and application thereof | |
| CN111545211A (en) | Graphene oxide-lanthanum oxide-cobalt hydroxide composite material, and synthesis method and application thereof | |
| CN111974424A (en) | Method for preparing magnetic dibromo-bismuth pentoxide composite photocatalytic material | |
| CN106517354A (en) | Nanometer alpha-phase iron oxide and preparation method thereof | |
| CN108404948B (en) | One kind (BiO)2CO3-BiO2-xComposite photocatalyst and preparation method and application thereof | |
| CN110422887A (en) | The preparation method of biomass-based magnetism hydro-thermal charcoal | |
| CN110227517A (en) | CuBi2O4/BiPO4P-n junction heterojunction photocatalyst, preparation method and applications | |
| Xue et al. | Construction of Cu 2+-doped CeO 2 nanocrystals hierarchical hollow structure and its enhanced photocatalytic performance |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20210323 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |