CN110102317A - MoS2-CeO2Compound and preparation method thereof - Google Patents
MoS2-CeO2Compound and preparation method thereof Download PDFInfo
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- CN110102317A CN110102317A CN201910295377.7A CN201910295377A CN110102317A CN 110102317 A CN110102317 A CN 110102317A CN 201910295377 A CN201910295377 A CN 201910295377A CN 110102317 A CN110102317 A CN 110102317A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 168
- 238000006243 chemical reaction Methods 0.000 claims abstract description 94
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims abstract description 76
- 150000001875 compounds Chemical class 0.000 claims abstract description 58
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000002604 ultrasonography Methods 0.000 claims abstract description 34
- 238000003756 stirring Methods 0.000 claims abstract description 31
- 238000005119 centrifugation Methods 0.000 claims abstract description 25
- 238000005406 washing Methods 0.000 claims abstract description 22
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000004202 carbamide Substances 0.000 claims abstract description 19
- 235000015393 sodium molybdate Nutrition 0.000 claims abstract description 19
- 239000011684 sodium molybdate Substances 0.000 claims abstract description 19
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 8
- 230000008569 process Effects 0.000 claims abstract description 6
- 229910002492 Ce(NO3)3·6H2O Inorganic materials 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 64
- 239000008367 deionised water Substances 0.000 claims description 18
- 229910021641 deionized water Inorganic materials 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 238000001354 calcination Methods 0.000 claims description 13
- 230000035484 reaction time Effects 0.000 claims description 6
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- 230000003197 catalytic effect Effects 0.000 abstract description 21
- 150000002466 imines Chemical class 0.000 abstract description 13
- 239000000126 substance Substances 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract 1
- 235000019441 ethanol Nutrition 0.000 description 28
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 24
- 229910052961 molybdenite Inorganic materials 0.000 description 22
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 18
- 239000003054 catalyst Substances 0.000 description 15
- 230000000694 effects Effects 0.000 description 15
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 13
- 239000001301 oxygen Substances 0.000 description 13
- 229910052760 oxygen Inorganic materials 0.000 description 13
- 230000015572 biosynthetic process Effects 0.000 description 11
- 239000000463 material Substances 0.000 description 10
- 238000003786 synthesis reaction Methods 0.000 description 10
- 239000002060 nanoflake Substances 0.000 description 7
- 238000006555 catalytic reaction Methods 0.000 description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 2
- 206010013786 Dry skin Diseases 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 239000012695 Ce precursor Substances 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 235000019445 benzyl alcohol Nutrition 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000007144 microwave assisted synthesis reaction Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002090 nanochannel Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
Classifications
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- 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
-
- 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
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
- B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C249/00—Preparation of compounds containing nitrogen atoms doubly-bound to a carbon skeleton
- C07C249/02—Preparation of compounds containing nitrogen atoms doubly-bound to a carbon skeleton of compounds containing imino groups
-
- 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
- Y02E60/50—Fuel cells
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The present invention relates to a kind of MoS2‑CeO2Compound and preparation method thereof, the specific steps are as follows: (1) take Ce (NO3)3·6H2O and PVP, is dissolved in ethylene glycol, stirs to clarify, and obtains solution A；(2) urea and PVP are taken, is dissolved in ethylene glycol, is stirred to clarify, solution B is obtained；(3) by after solution A and solution B hybrid reaction, after washing, drying, CeO is obtained2；(4) by CeO obtained in step (3)2It is dissolved in ethylene glycol with sodium molybdate and thiocarbamide, is reacted after ultrasound, after reaction, washing, ultrasound, centrifugation, drying obtain MoS2‑CeO2Compound.Compared with prior art, the present invention can be made different compounds, the catalytic effect of imine reaction is especially apparent, entire process route is easy, low energy consumption, obtained MoS easily by adjusting the ratio of each substance2‑CeO2Compound yield is high, and combining case is preferable.
Description
Technical field
The present invention relates to a kind of compounds and preparation method thereof, more particularly, to a kind of MoS2-CeO2Compound and its preparation
Method.
Background technique
In recent years, CeO2Carrier and some other Material claddings are widely used as at novel with unique properties
Compound, it is unique and excellent oxygen storage capacity has become research hotspot.CeO2As a kind of important rare earth oxide,
It is widely used in the technical fields such as catalysis, optics, electrochemistry and Environmental Chemistry.CeO2The defect on surface is mainly by oxygen sky
Caused by position, in few oxygen environment, CeO2A large amount of Lacking oxygen can be formed, oxygen is released into environment；In oxygen-enriched environment,
CeO2It can achieve the purpose that store oxygen by Lacking oxygen again, so CeO2Ability with excellent release, storage oxygen.Due to
Single CeO2Catalytic effect is lower, single property, it is necessary to the certain compounds of some other materials synthesis, keep it multi-party
Face efficient plays a role.MoS2It is typical stratiform transistion metal compound, MoS2Show good catalysis and electricity
Performance, more and more attention has been paid to application.In addition, molybdenum disulfide nano sheet itself has biggish specific surface area, show good
Good adsorptivity, however for molybdenum disulfide and the fresh few research of the compound aspect of other materials, especially with CeO2It is compound.Herein
CeO is synthesized using hydro-thermal method2, because it is not only easy to operate, but also can produce the product with excellent properties.
Up to the present, related CeO2The report of nano flake is seldom, and it is most of be all some large scales or with
Some other metal material is combined, and synthesizes some composite fuel batteries or some photochemical catalysts, CeO2Nano flake
Large scale and thin layer are still awaiting development.
Chinese patent CN106636824A discloses a kind of CeO2+MoS2The fuel cell high capacity hydrogen storage of composite catalyzing
Alloy and preparation method thereof, but CeO is not related to2+MoS2Preparation method.
Summary of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of MoS2-CeO2It is compound
Object and preparation method thereof.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of MoS2-CeO2Compound and preparation method thereof, the specific steps are as follows:
(1) Ce (NO is taken3)3·6H2O and PVP, is dissolved in ethylene glycol, stirs to clarify, and obtains solution A；
(2) urea and PVP are taken, is dissolved in ethylene glycol, is stirred to clarify, solution B is obtained；
(3) by after solution A and solution B hybrid reaction, after washing, drying, CeO is obtained2；
(4) by CeO obtained in step (3)2It is dissolved in ethylene glycol with sodium molybdate and thiocarbamide, is reacted after ultrasound, reaction knot
Shu Hou, washing, ultrasound, centrifugation, drying, obtains MoS2-CeO2Compound.
Preferably, in step (1): Ce (NO3)3·6H2O, the proportion of PVP and ethylene glycol is (1-30) g:(1-10) g:
(20-200)ml。
Preferably, in step (2): the proportion of urea, PVP and ethylene glycol is (1-20) g:(10-80) g:(2-200) mL.
Preferably, the process conditions reacted in step (3) are as follows: 160-220 DEG C of reaction temperature, reaction time 2-8h.
Preferably, in step (3) the step of washing are as follows: deionized water, EtOH Sonicate, centrifugation are successively used, it is each to clean 3 times,
Ultrasonic time is 10-40min, centrifugation time 2-10min, revolving speed 5000-10000rpm.
Preferably, to obtained CeO in step (3)2It is calcined, the process conditions of calcining are as follows: 400-800 DEG C in air
Calcine 1-3h.The CeO obtained after calcining2Than the CeO without calcining2, performance is good, and it is solvent-free and other impurities, it is calcined
CeO2Storage oxygen and release performance it is stronger, with MoS2After material progress is compound, oxygen and release performance enhancing are stored up.
Preferably, in step (3): dry to use vacuum oven, drying temperature is 50-80 DEG C, drying time 12-
24h。
Preferably, in step (4): the CeO of addition2Amount, with Na2MoO4-CeO2Different mol ratio, calculate each substance
The compound of different ratio can be obtained with this for dosage.
Preferably, in step (4): the molar ratio of sodium molybdate and thiocarbamide is (0.5-3): (1-10).
Preferably, in step (4): ultrasonic time is 10-40min before reacting, and reaction temperature is 160-220 DEG C, when reaction
Between be 12-24h.
Preferably, in step (4): successively using deionized water, EtOH Sonicate, centrifugation, each cleaning 3 times, ultrasonic time 10-
40min, centrifugation time 2-10min, revolving speed 5000-10000rpm.
During the preparation process, if material additive amount is excessive or very few, the purity of the material of formation, yield be will receive
It influences.Temperature is too low or too high, perhaps the too short material property to be formed that will cause is reduced or cannot be synthesized overlong time
Target material.
The present invention utilizes CeO2Special property, as substrate, with a certain amount of MoS2It is compound, it is formed a kind of novel
Catalyst, catalytic efficiency is significantly larger than the catalytic efficiency of homogenous material.Using hydro-thermal method, the MoS of different proportion is prepared2/
CeO2Novel complexes, catalytic effect is significant, is higher than general compound, with CeO2-MoS2- ca (1:2) compound is catalyst
It is 106.109mmolg- that best imines conversion ratio, which occurs, in system1h-1, be higher than bibliography (H.Ding, J.Yang, S.Ma,
N.Yigit,J.Xu,G.Rupprechter,J.Wang,Large Dimensional CeO2Nanoflakes by
Microwave-Assisted Synthesis:Lamellar Nano-Channels and Surface Oxygen
Vacancies Promote Catalytic Activity, ChemCatChem, 10 (2018) 4100-4108.) in 50 DEG C
When 9.52mmolg-1h-1Sample and bibliography (J.Zhang, J.Yang, J.Wang, H.Ding, Q.Liu,
U.Schubert,Y.Rui,J.Xu,Surface oxygen vacancies dominated CeO2as efficient
catalyst for imine synthesis:Influences of different cerium precursors,
Molecular Catalysis, 443 (2017) 131-138.) in 50 DEG C when 4.9mmolg-1h-1Sample.
Herein with CeO2For substrate, with a certain amount of MoS2It is combined into the novel compound with strong oxidizing property, it is in high temperature
Under the conditions of (120 DEG C), break conventional low-temperature catalyzed, the reaction time is short, and catalytic efficiency is previously reported highest imines
10 times of (106.109mmolg of catalytic conversion-1h-1)。
The MoS that the present invention is prepared2-CeO2Compound chemical property is stable and has stronger catalytic activity, is higher than one
As 10 times of same type compound or more, therefore as a kind of low cost, the catalyst of high catalytic performance, instead of some high costs,
The compound of low catalytic performance.
Compared with prior art, the invention has the following advantages:
(1)MoS2-CeO2Compound provides a kind of higher complex catalyst of catalytic performance, breaks Conventional cryogenic and urges
Change, the low situation of catalytic efficiency；
(2)MoS2-CeO2Compound preparation method process route is simple, and cost of material is low；
(3)MoS2-CeO2Compound has played significant role, may replace general catalyst in imines catalysis, applies
In reaction, greatly promote its reaction rate.
Detailed description of the invention
Fig. 1 is the MoS being prepared2-CeO2The XRD spectra of compound；
Fig. 2 is the CeO being prepared in embodiment 72-MoS2- ca (2:1) compound field emission scanning electron microscope figure；
Fig. 3 is the CeO being prepared in embodiment 82-MoS2- ca (1:1) compound field emission scanning electron microscope figure；
Fig. 4 is the CeO being prepared in embodiment 102-MoS2- ca (1:5) compound field emission scanning electron microscope figure；
Fig. 5 is different MoS2-CeO2The result figure of the conversion ratio of complex catalysts imine reaction；
Fig. 6 is the MoS prepared in embodiment 1-42-CeO2The conversion ratio of complex catalysts imine reaction and reaction time
Graph of relation；
Fig. 7 is the MoS prepared in embodiment 4,8,112-CeO2Complex catalysts imine reaction and individual MoS2、CeO2
It is catalyzed the conversion ratio and the graph of relation in reaction time of imine reaction.
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
In embodiment: first a in aa indicates the compound of synthesis, when synthesis CeO used2It is without calcining
, second a indicates synthesized CeO2-MoS2(x:y) compound, without calcination processing；
First a in ca indicates the compound of synthesis, when synthesis CeO used2It is to be calcined by (500 DEG C) of high temperature
, second a indicates synthesized CeO2-MoS2(x:y) compound, without calcination processing；
A in ac indicates the compound of synthesis, when synthesis CeO used2It is without calcining, c indicates synthesized
CeO2-MoS2(x:y) compound, at 540 DEG C, calcining obtains for 1 hour.
Embodiment 1
MoS2-CeO2Compound the preparation method is as follows:
(1) Ce (NO is taken3)3·6H2O (2.17g) and PVP (0.5g) is dissolved in the EG (ethylene glycol) of 20mL, stirs to clarify.
Urea (0.45g) and PVP (0.5g) are weighed simultaneously, is dissolved in 15mL EG, stirs to clarify.Then two solution are sufficiently mixed,
It is transferred to reaction kettle, at 190 DEG C, after reacting 6h, is washed three times, is then placed in vacuum oven with ethyl alcohol, 60 DEG C of dryings
12h obtains CeO2；
(2) CeO obtained in step (1) is taken2(0.516g), it is sufficiently mixed with sodium molybdate (0.036g), thiocarbamide (0.057g)
It is even, it is dissolved with the EG of 50mL, ultrasound is transferred in reaction kettle after 30 minutes, and reaction controlling is at 200 DEG C, and reaction is for 24 hours；
(3) to after reaction, respectively washed three times repeatedly with deionized water and ethyl alcohol, using ultrasound and centrifugation, reach compared with
Good washing effect, is finally putting into vacuum oven, 60 DEG C of dry 12h are to get MoS2-CeO2- aa (20:1) compound.
Embodiment 2
(1) Ce (NO is taken3)3·6H2O (2.17g) and PVP (0.5g), is dissolved in the EG of 20mL, stirs to clarify.It weighs simultaneously
Urea (0.45g) and PVP (0.5g), are dissolved in 15mL EG, stir to clarify.Then two solution are sufficiently mixed, are transferred to anti-
Kettle is answered, at 190 DEG C, after reacting 6h, is washed three times, is then placed in vacuum oven with ethyl alcohol, 60 DEG C of dry 12h are obtained
CeO2；
(2) CeO obtained in step (1) is taken2(0.516g), it is sufficiently mixed with sodium molybdate (0.145g), thiocarbamide (0.228g)
It is even, it is dissolved with the EG of 50mL, ultrasound is transferred in reaction kettle after 30 minutes, and reaction controlling is at 200 DEG C, and reaction is for 24 hours；
(3) to after reaction, respectively washed three times repeatedly with deionized water and ethyl alcohol, using ultrasound and centrifugation, reach compared with
Good washing effect, is finally putting into vacuum oven, 60 DEG C of dry 12h are to get MoS2-CeO2- aa (5:1) compound
Embodiment 3
(1) Ce (NO is taken3)3·6H2O (2.17g) and PVP (0.5g), is dissolved in the EG of 20mL, stirs to clarify.It weighs simultaneously
Urea (0.45g) and PVP (0.5g), are dissolved in 15mL EG, stir to clarify.Then two solution are sufficiently mixed, are transferred to anti-
Kettle is answered, at 190 DEG C, after reacting 6h, is washed three times, is then placed in vacuum oven with ethyl alcohol, 60 DEG C of dry 12h are obtained
CeO2；
(2) CeO obtained in step (1) is taken2(0.516g), it is sufficiently mixed with sodium molybdate (0.363g), thiocarbamide (0.570g)
It is even, it is dissolved with the EG of 50mL, ultrasound is transferred in reaction kettle after 30 minutes, and reaction controlling is at 200 DEG C, and reaction is for 24 hours；
(3) to after reaction, respectively washed three times repeatedly with deionized water and ethyl alcohol, using ultrasound and centrifugation, reach compared with
Good washing effect, is finally putting into vacuum oven, 60 DEG C of dry 12h are to get MoS2-CeO2- aa (2:1) compound.
Embodiment 4
(1) Ce (NO is taken3)3·6H2O (2.17g) and PVP (0.5g), is dissolved in the EG of 20mL, stirs to clarify.It weighs simultaneously
Urea (0.45g) and PVP (0.5g), are dissolved in 15mL EG, stir to clarify.Then two solution are sufficiently mixed, are transferred to anti-
Kettle is answered, at 190 DEG C, after reacting 6h, is washed three times, is then placed in vacuum oven with ethyl alcohol, 60 DEG C of dry 12h are obtained
CeO2；
(2) CeO obtained in step (1) is taken2(0.516g), it is sufficiently mixed with sodium molybdate (0.725g), thiocarbamide (1.141g)
It is even, it is dissolved with the EG of 50mL, ultrasound is transferred in reaction kettle after 30 minutes, and reaction controlling is at 200 DEG C, and reaction is for 24 hours；
(3) to after reaction, respectively washed three times repeatedly with deionized water and ethyl alcohol, using ultrasound and centrifugation, reach compared with
Good washing effect, is finally putting into vacuum oven, 60 DEG C of dry 12h are to get MoS2-CeO2- aa (1:1) compound
Embodiment 5
(1) Ce (NO is taken3)3·6H2O (2.17g) and PVP (0.5g), is dissolved in the EG of 20mL, stirs to clarify.It weighs simultaneously
Urea (0.45g) and PVP (0.5g), are dissolved in 15mL EG, stir to clarify.Then two solution are sufficiently mixed, are transferred to anti-
Kettle is answered, at 190 DEG C, after reacting 6h, is washed three times, is then placed in vacuum oven with ethyl alcohol, 60 DEG C of dry 12h are obtained
CeO2, then place in Muffle furnace, calcine 1h at 500 DEG C of high temperature, obtain c-CeO2；
(2) CeO obtained in step (1) is taken2(0.516g), it is sufficiently mixed with sodium molybdate (0.036mg), thiocarbamide (0.057g)
It is even, it is dissolved with the EG of 50mL, ultrasound is transferred in reaction kettle after 30 minutes, and reaction controlling is at 200 DEG C, and reaction is for 24 hours；
(3) to after reaction, respectively washed three times repeatedly with deionized water and ethyl alcohol, using ultrasound and centrifugation, reach compared with
Good washing effect, is finally putting into vacuum oven, 60 DEG C of dry 12h are to get MoS2-CeO2- ca (20:1) compound.
Embodiment 6
(1) Ce (NO is taken3)3·6H2O (2.17g) and PVP (0.5g), is dissolved in the EG of 20mL, stirs to clarify.It weighs simultaneously
Urea (0.45g) and PVP (0.5g), are dissolved in 15ml EG, stir to clarify.Then two solution are sufficiently mixed, are transferred to anti-
Kettle is answered, at 190 DEG C, after reacting 6h, is washed three times, is then placed in vacuum oven with ethyl alcohol, 60 DEG C of dry 12h are obtained
CeO2, then place in Muffle furnace, calcine 1h at 500 DEG C of high temperature, obtain c-CeO2；
(2) CeO obtained in step (1) is taken2(0.516g), it is sufficiently mixed with sodium molybdate (0.145g), thiocarbamide (0.228g)
It is even, it is dissolved with the EG of 50mL, ultrasound is transferred in reaction kettle after 30 minutes, and reaction controlling is at 200 DEG C, and reaction is for 24 hours；
(3) to after reaction, respectively washed three times repeatedly with deionized water and ethyl alcohol, using ultrasound and centrifugation, reach compared with
Good washing effect, is finally putting into vacuum oven, 60 DEG C of dry 12h are to get MoS2-CeO2- ca (5:1) compound.
Embodiment 7
(1) Ce (NO is taken3)3·6H2O (2.17g) and PVP (0.5g), is dissolved in the EG of 20mL, stirs to clarify.It weighs simultaneously
Urea (0.45g) and PVP (0.5g), are dissolved in 15mL EG, stir to clarify.Then two solution are sufficiently mixed, are transferred to anti-
Kettle is answered, at 190 DEG C, after reacting 6h, is washed three times, is then placed in vacuum oven with ethyl alcohol, 60 DEG C of dry 12h are obtained
CeO2, then place in Muffle furnace, calcine 1h at 500 DEG C of high temperature, obtain c-CeO2；
(2) CeO obtained in step (1) is taken2(0.516g), it is sufficiently mixed with sodium molybdate (0.363g), thiocarbamide (0.570g)
It is even, it is dissolved with the EG of 50ml, ultrasound is transferred in reaction kettle after 30 minutes, and reaction controlling is at 200 DEG C, and reaction is for 24 hours；
(3) to after reaction, respectively washed three times repeatedly with deionized water and ethyl alcohol, using ultrasound and centrifugation, reach compared with
Good washing effect, is finally putting into vacuum oven, 60 DEG C of dry 12h are to get MoS2-CeO2- ca (2:1) compound.
Embodiment 8
(1) Ce (NO is taken3)3·6H2O (2.17g) and PVP (0.5g), is dissolved in the EG of 20mL, stirs to clarify.It weighs simultaneously
Urea (0.45g) and PVP (0.5g), are dissolved in 15mL EG, stir to clarify.Then two solution are sufficiently mixed, are transferred to anti-
Kettle is answered, at 190 DEG C, after reacting 6h, is washed three times, is then placed in vacuum oven with ethyl alcohol, 60 DEG C of dry 12h are obtained
CeO2, then place in Muffle furnace, calcine 1h at 500 DEG C of high temperature, obtain c-CeO2；
(2) CeO obtained in step (1) is taken2(0.516g), it is sufficiently mixed with sodium molybdate (0.725g), thiocarbamide (1.141g)
It is even, it is dissolved with the EG of 50mL, ultrasound is transferred in reaction kettle after 30 minutes, and reaction controlling is at 200 DEG C, and reaction is for 24 hours；
(3) to after reaction, respectively washed three times repeatedly with deionized water and ethyl alcohol, using ultrasound and centrifugation, reach compared with
Good washing effect, is finally putting into vacuum oven, 60 DEG C of dry 12h are to get MoS2-CeO2- ca (1:1) compound.
Embodiment 9
(1) Ce (NO is taken3)3·6H2O (2.17g) and PVP (0.5g), is dissolved in the EG of 20mL, stirs to clarify.It weighs simultaneously
Urea (0.45g) and PVP (0.5g), are dissolved in 15mL EG, stir to clarify.Then two solution are sufficiently mixed, are transferred to anti-
Kettle is answered, at 190 DEG C, after reacting 6h, is washed three times, is then placed in vacuum oven with ethyl alcohol, 60 DEG C of dry 12h are obtained
CeO2It then places in Muffle furnace, calcines 1h at 500 DEG C of high temperature, obtain c-CeO2；
(2) CeO obtained in step (1) is taken2(0.516g), it is sufficiently mixed with sodium molybdate (1.451g), thiocarbamide (2.28g)
It is even, it is dissolved with the EG of 50mL, ultrasound is transferred in reaction kettle after 30 minutes, and reaction controlling is at 200 DEG C, and reaction is for 24 hours；
(3) to after reaction, respectively washed three times repeatedly with deionized water and ethyl alcohol, using ultrasound and centrifugation, reach compared with
Good washing effect, is finally putting into vacuum oven, 60 DEG C of dry 12h are to get MoS2-CeO2- ca (1:2) compound.
Embodiment 10
(1) Ce (NO is taken3)3·6H2O (2.17g) and PVP (0.5g), is dissolved in the EG of 20mL, stirs to clarify.It weighs simultaneously
Urea (0.45g) and PVP (0.5g), are dissolved in 15mL EG, stir to clarify.Then two solution are sufficiently mixed, are transferred to anti-
Kettle is answered, at 190 DEG C, after reacting 6h, is washed three times, is then placed in vacuum oven with ethyl alcohol, 60 DEG C of dry 12h are obtained
CeO2, then place in Muffle furnace, calcine 1h at 500 DEG C of high temperature, obtain c-CeO2；
(2) CeO obtained in step (1) is taken2(0.516g), it is sufficiently mixed with sodium molybdate (3.629g), thiocarbamide (5.079mg)
It is even, it is dissolved with the EG of 50mL, ultrasound is transferred in reaction kettle after 30 minutes, and reaction controlling is at 200 DEG C, and reaction is for 24 hours；
(3) to after reaction, respectively washed three times repeatedly with deionized water and ethyl alcohol, using ultrasound and centrifugation, reach compared with
Good washing effect, is finally putting into vacuum oven, 60 DEG C of dry 12h are to get MoS2-CeO2- ca (1:5) compound.
Embodiment 11
(1) Ce (NO is taken3)3·6H2O (2.17g) and PVP (0.5g), is dissolved in the EG of 20mL, stirs to clarify.It weighs simultaneously
Urea (0.45g) and PVP (0.5g), are dissolved in 15mL EG, stir to clarify.Then two solution are sufficiently mixed, are transferred to anti-
Kettle is answered, at 190 DEG C, after reacting 6h, is washed three times, is then placed in vacuum oven with ethyl alcohol, 60 DEG C of dry 12h are obtained
CeO2, then place in Muffle furnace, calcine 1h at 500 DEG C of high temperature, obtain c-CeO2；
(2) CeO obtained in step (1) is taken2(0.516g), it is sufficiently mixed with sodium molybdate (0.725g), thiocarbamide (1.141mg)
It is even, it is dissolved with the EG of 50mL, ultrasound is transferred in reaction kettle after 30 minutes, and reaction controlling is at 200 DEG C, and reaction is for 24 hours；
(3) to after reaction, respectively washed three times repeatedly with deionized water and ethyl alcohol, using ultrasound and centrifugation, reach compared with
Good washing effect, is finally putting into vacuum oven, 60 DEG C of dry 12h, then places in Muffle furnace, in the protection of argon gas
Under, 1h is calcined at 500 DEG C of high temperature to get MoS2-CeO2- cc (1:1) compound.
Embodiment 12
(1) Ce (NO is taken3)3·6H2O (2.17g) and PVP (0.5g), is dissolved in the EG of 20mL, stirs to clarify.It weighs simultaneously
Urea (0.45g) and PVP (0.5g), are dissolved in 15mL EG, stir to clarify.Then two solution are sufficiently mixed, are transferred to anti-
Kettle is answered, at 190 DEG C, after reacting 6h, is washed three times, is then placed in vacuum oven with ethyl alcohol, 60 DEG C of dry 12h are obtained
CeO2；
(2) CeO obtained in step (1) is taken2(0.516g), it is sufficiently mixed with sodium molybdate (0.725g), thiocarbamide (1.141g)
It is even, it is dissolved with the EG of 50mL, ultrasound is transferred in reaction kettle after 30 minutes, and reaction controlling is at 200 DEG C, and reaction is for 24 hours；
(3) to after reaction, respectively washed three times repeatedly with deionized water and ethyl alcohol, using ultrasound and centrifugation, reach compared with
Good washing effect, is finally putting into vacuum oven, 60 DEG C of dry 12h, then places in Muffle furnace, forges at 500 DEG C of high temperature
1h is burnt to get MoS2-CeO2- ac (1:1) compound.
Embodiment 13
(1) Ce (NO is taken3)3·6H2O (3g) and PVP (1g), is dissolved in the EG of 20mL, stirs to clarify.Urea is weighed simultaneously
(2g) and PVP (8g), is dissolved in 20mL EG, stirs to clarify.Then two solution are sufficiently mixed, are transferred to reaction kettle,
At 160 DEG C, after reacting 8h, is washed three times, be then placed in vacuum oven with ethyl alcohol, 50 DEG C of dryings for 24 hours, obtain CeO2；
(2) CeO obtained in step (1) is taken2(0.516g), it is sufficiently mixed with sodium molybdate (0.618g), thiocarbamide (0.761g)
It is even, it is dissolved with the EG of 50mL, ultrasound is transferred in reaction kettle after 30 minutes, and reaction controlling reacts 12h at 220 DEG C；
(3) to after reaction, respectively washed three times repeatedly with deionized water and ethyl alcohol, using ultrasound and centrifugation, reach compared with
Good washing effect, is finally putting into vacuum oven, 60 DEG C of dry 12h are to get MoS2-CeO2Compound.
Embodiment 14
(1) Ce (NO is taken3)3·6H2O (1g) and PVP (5g), is dissolved in the EG of 20mL, stirs to clarify.Urea is weighed simultaneously
(0.1g) and PVP (1g), is dissolved in 0.2mL EG, stirs to clarify.Then two solution are sufficiently mixed, are transferred to reaction kettle,
At 220 DEG C, after reacting 2h, is washed three times, be then placed in vacuum oven with ethyl alcohol, 80 DEG C of dry 18h obtain CeO2；
(2) CeO obtained in step (1) is taken2(0.516g), it is sufficiently mixed with sodium molybdate (0.103g), thiocarbamide (0.076g)
It is even, it is dissolved with the EG of 50mL, ultrasound is transferred in reaction kettle after 30 minutes, and reaction controlling reacts 18h at 160 DEG C；
(3) to after reaction, respectively washed three times repeatedly with deionized water and ethyl alcohol, using ultrasound and centrifugation, reach compared with
Good washing effect, is finally putting into vacuum oven, 60 DEG C of dry 12h are to get MoS2-CeO2Compound.
The MoS that will be prepared2-CeO2Compound is used for imines synthetic reaction, and equation is as follows:
Specific steps are as follows: take benzyl alcohol (10mmol) and aniline (20mmol), CeO is added2-MoS2Compound catalyst
(50mg) after mixing, is stirred under 120 DEG C of oil baths, and every two hour takes a sample, take altogether 5 times (the last one sampling, and it is preceding
Primary sample is spaced 4 hours), by HPLC, response situation is detected, reaction rate, conversion ratio and selectivity are calculated, to compare
That composite material catalytic performance is preferable.
Fig. 1 is the CeO being prepared2-MoS2The XRD spectra of compound, prepared MoS2(MoS2- a) nano flake is aobvious
Almost unbodied structure is shown, shows MoS2The crystallinity of-a is low.The CeO of calcining2- c nano flake shows typical CeO2
Crystalline phase (JCPDF No:34-0394).CeO2-MoS2The compound of-ca (1:2) is shown and pure CeO2- c is almost the same
XRD diagram case.The CeO of different proportion2-MoS2- ca composite material exhibits go out similar as a result, but due to surface MoS2It is more, CeO2
(111) peak intensity of phase reduces.
Fig. 2-4 is respectively the SEM data of embodiment 7,8,10, such as schemes MoS2- a and CeO2- c shows nano flake knot
Structure works as CeO2- c nano flake and MoS2When-a is combined in certain proportion, sheet structure still can be protected with more thick-layer structure
It deposits, the CeO of other ratios2-MoS2- ca has similar form, works as CeO2Proportion is suitable when large, Material cladding compared with
It is good, it is similar to spherical shape, lamella is less, and catalytic performance is also preferable.
Fig. 5 is to be catalyzed imines synthetic reaction for the compound (25mmol) synthesized under different condition under different temperatures
Conversion ratio obtained by (12h).As seen from the figure, at 60 DEG C, the catalytic effect of compound is far below compound under the conditions of 120 DEG C
Catalytic effect, CeO2-MoS2- ac (2:1) (Ar) refers under protection of argon gas, CeO2-MoS2- ac (2:1) is at 540 DEG C, calcining 1
Hour.CeO2-MoS2- ac (2:1) (Air) refers in air, CeO2-MoS2- ac (2:1) is calcined 1 hour at 540 DEG C.
CeO2-MoS2- aa (2:1) refers to the compound of non-calcination processing, finally finds CeO2-MoS2The catalysis of-aa (2:1) compound is imitated
Fruit is best.
Fig. 6 is the compound (25mmol) of different proportion, at 120 DEG C, conversion obtained by catalysis imines synthetic reaction (12h)
Rate.By comparing the compound of 4 kinds of different proportions synthesis, CeO is found2-MoS2The conversion ratio of-aa (1:1) complex catalysts reaction
Highest illustrates that its catalytic effect is best, CeO2-MoS2The conversion ratio of-aa (20:1) complex catalysts reaction is minimum, illustrates to synthesize
Compound in CeO2Content is excessive, will affect catalytic effect.
Fig. 7 is the compound (25mmol) synthesized under different conditions, at 120 DEG C, is catalyzed imines synthetic reaction (12h) institute
Conversion ratio is obtained, by comparing the compound synthesized under 3 kinds of different conditions, finds CeO2-MoS2The reaction of-ca (1:1) complex catalysts
Conversion ratio highest, catalytic effect is best, illustrates in the compound of synthesis with the CeO after high-temperature calcination2, catalyst can be reinforced
Catalytic capability, promote CeO2In Ce3+It is transferred to Ce4+And promote in the environment from O2It generates active oxygen atom (O*), makes it
Catalytic effect is more preferable.
The above description of the embodiments is intended to facilitate ordinary skill in the art to understand and use the invention.
Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein general
Principle is applied in other embodiments without having to go through creative labor.Therefore, the present invention is not limited to the above embodiments, ability
Field technique personnel announcement according to the present invention, improvement and modification made without departing from the scope of the present invention all should be of the invention
Within protection scope.
Claims (10)
1. a kind of MoS2-CeO2The preparation method of compound, which is characterized in that specific step is as follows:
(1) Ce (NO is taken3)3·6H2O and PVP, is dissolved in ethylene glycol, stirs to clarify, and obtains solution A；
(2) urea and PVP are taken, is dissolved in ethylene glycol, is stirred to clarify, solution B is obtained；
(3) by after solution A and solution B hybrid reaction, after washing, drying, CeO is obtained2；
(4) by CeO obtained in step (3)2It is dissolved in ethylene glycol with sodium molybdate and thiocarbamide, is reacted after ultrasound, after reaction,
Washing, ultrasound, centrifugation, drying, obtain MoS2-CeO2Compound.
2. a kind of MoS according to claim 12-CeO2The preparation method of compound, which is characterized in that in step (1): Ce
(NO3)3·6H2O, the proportion of PVP and ethylene glycol is (1-30) g:(1-10) g:(20-200) ml.
3. a kind of MoS according to claim 12-CeO2Compound and preparation method thereof, which is characterized in that in step (2):
The proportion of urea, PVP and ethylene glycol is (1-20) g:(10-80) g:(2-200) ml.
4. a kind of MoS according to claim 12-CeO2The preparation method of compound, which is characterized in that anti-in step (3)
The process conditions answered are as follows: 160-220 DEG C of reaction temperature, reaction time 2-8h.
5. a kind of MoS according to claim 12-CeO2The preparation method of compound, which is characterized in that step is washed in (3)
The step of washing are as follows: successively use deionized water, EtOH Sonicate, centrifugation, each cleaning 3 times, ultrasonic time 10-40min, centrifugation time
For 2-10min, revolving speed 5000-10000rpm.
6. a kind of MoS according to claim 12-CeO2The preparation method of compound, which is characterized in that right in step (3)
Obtained CeO2It is calcined, the process conditions of calcining are as follows: 400-800 DEG C of calcining 1-3h in air.
7. a kind of MoS according to claim 12-CeO2The preparation method of compound, which is characterized in that in step (3): dry
Dry to use vacuum oven, drying temperature is 50-80 DEG C, drying time 12-24h.
8. a kind of MoS according to claim 12-CeO2Compound and preparation method thereof, which is characterized in that in step (4):
The molar ratio of sodium molybdate and thiocarbamide is (0.5-3): (1-10).
9. a kind of MoS according to claim 12-CeO2The preparation method of compound, which is characterized in that in step (4): anti-
Ultrasonic time is 10-40min before answering, and reaction temperature is 160-220 DEG C, reaction time 12-24h.
10. a kind of MoS according to claim 12-CeO2The preparation method of compound, which is characterized in that in step (4):
Deionized water, EtOH Sonicate, centrifugation are successively used, it is each to clean 3 times, ultrasonic time 10-40min, centrifugation time 2-10min,
Revolving speed is 5000-10000rpm.
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| CN112062162A (en) * | 2020-09-18 | 2020-12-11 | 浙江理工大学 | MnFe2O4@MoS2Lamellar spherical magnetic composite material and preparation method thereof |
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| CN115554975A (en) * | 2022-10-13 | 2023-01-03 | 中南大学 | Adsorbing material and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112062162A (en) * | 2020-09-18 | 2020-12-11 | 浙江理工大学 | MnFe2O4@MoS2Lamellar spherical magnetic composite material and preparation method thereof |
| CN115180739A (en) * | 2022-07-18 | 2022-10-14 | 威海智洁环保技术有限公司 | Method for removing 2-methylisoborneol and geosmin in drinking water |
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| CN115554975A (en) * | 2022-10-13 | 2023-01-03 | 中南大学 | Adsorbing material and preparation method and application thereof |
| CN115554975B (en) * | 2022-10-13 | 2023-07-21 | 中南大学 | Adsorption material and preparation method and application thereof |
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