CN107233900A - A kind of molybdenum disulfide composite nano-gold photochemical catalyst and preparation method thereof - Google Patents
A kind of molybdenum disulfide composite nano-gold photochemical catalyst and preparation method thereof Download PDFInfo
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- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 83
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 239000010931 gold Substances 0.000 title claims abstract description 51
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 34
- 239000003054 catalyst Substances 0.000 title claims abstract description 33
- 239000002131 composite material Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000000243 solution Substances 0.000 claims abstract description 30
- 239000002105 nanoparticle Substances 0.000 claims abstract description 27
- 238000003756 stirring Methods 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000008367 deionised water Substances 0.000 claims abstract description 22
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 22
- 239000002245 particle Substances 0.000 claims abstract description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 101710116850 Molybdenum cofactor sulfurase 2 Proteins 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 16
- 239000011259 mixed solution Substances 0.000 claims abstract description 15
- 239000001509 sodium citrate Substances 0.000 claims abstract description 14
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims abstract description 14
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 12
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910000077 silane Inorganic materials 0.000 claims abstract description 8
- 239000000084 colloidal system Substances 0.000 claims abstract description 7
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000011941 photocatalyst Substances 0.000 claims abstract description 6
- 229910052961 molybdenite Inorganic materials 0.000 claims description 26
- 235000015393 sodium molybdate Nutrition 0.000 claims description 15
- DLFVBJFMPXGRIB-UHFFFAOYSA-N Acetamide Chemical compound CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000013049 sediment Substances 0.000 claims description 12
- 239000011684 sodium molybdate Substances 0.000 claims description 12
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 11
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 11
- 235000013339 cereals Nutrition 0.000 claims description 9
- 229910004042 HAuCl4 Inorganic materials 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 238000005245 sintering Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 235000007164 Oryza sativa Nutrition 0.000 claims description 3
- 239000004567 concrete Substances 0.000 claims description 3
- 235000009566 rice Nutrition 0.000 claims description 3
- 240000007594 Oryza sativa Species 0.000 claims 1
- 235000019441 ethanol Nutrition 0.000 claims 1
- 125000000446 sulfanediyl group Chemical group *S* 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 4
- 238000007146 photocatalysis Methods 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract 1
- 235000005979 Citrus limon Nutrition 0.000 description 5
- 244000131522 Citrus pyriformis Species 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 238000003980 solgel method Methods 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- -1 constant temperature Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000003643 water by type Substances 0.000 description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- 241000209094 Oryza Species 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000002079 cooperative effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 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
- 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
-
- B01J35/39—
Abstract
It is that the composite photo-catalyst obtained on spherical molybdenum disulfide nano particle is uniformly compounded in by gold nano grain the invention discloses a kind of molybdenum disulfide composite nano-gold photochemical catalyst.Its preparation method is：1) spherical molybdenum disulfide nano particle is prepared using chemical synthesis；2) weigh step 1) prepared by nanometer MOS 2 particle be scattered in the mixed solution of deionized water and absolute ethyl alcohol, add silane coupler, stirring draws appropriate HAuCl to well mixed4Solution is simultaneously added dropwise in mixed solution, after being well mixed, adds and 30 40min are stirred under sodium citrate solution, constant temperature, obtain colloid, centrifuge and wash, and is circulated three times, is dried in drying box, is produced molybdenum disulfide composite nano-gold photochemical catalyst.The present invention has prepared molybdenum disulfide composite nano-gold photochemical catalyst using sol-gal process, can increase the avtive spot between Au nano-particles and molybdenum disulfide, so as to improve photocatalysis performance.
Description
Technical field
The invention belongs to technical field of nano-composite photocatalyst, a kind of molybdenum disulfide composite nano-gold is more particularly related to
Photochemical catalyst and preparation method thereof.
Background technology
Photocatalysis technology so that its is easy to operate, pollution-free, can directly utilize the advantages of sunshine and turn into current Solar use
Grind one of the focus that makes internal disorder or usurp.Photocatalysis technology based on semi-conducting material is in purification water pollution, organic synthesis and photolysis water hydrogen etc.
The utilization aspect of environment and resource has important application, is a kind of efficient, low energy consumption, cleaning, the technology of non-secondary pollution.
In catalyticing research and application direction, physicochemical properties unique nanometer Au have caused the concern of researcher.Receive
It is more prominent that the cooperative effect of rice Au and carrier makes that Au catalytic activity show, and current photocatalysis focuses mostly in TiO in studying2、
CeO2Etc. traditional loaded catalyst.
Different energy gaps are presented because the crystal number of plies is different in molybdenum disulfide, wherein the energy gap of multilayer molybdenum disulfide
For 1.2eV, the energy gap of individual layer molybdenum disulfide is 1.8eV.Molybdenum disulfide is a kind of semi-conducting material of function admirable, simultaneously
As a kind of transition metal stratiform sulfide, because the performances such as its good optics, electricity, lubrication and catalyst cause people
Extensive concern.The molybdenum disulfide marginal texture of Nano grade is complicated, with very high unsaturation, and reactivity is high, in light
Catalyst field causes the extensive concern of people.
The content of the invention
It is an object of the invention to provide a kind of molybdenum disulfide composite nano-gold photochemical catalyst and preparation method thereof, so as to obtain
The photochemical catalyst that the higher nanometer Au of catalytic activity is combined with molybdenum disulfide.
The present invention is achieved in that a kind of molybdenum disulfide composite nano-gold photochemical catalyst, is uniform by gold nano grain
It is compounded in the composite photo-catalyst obtained on spherical molybdenum disulfide nano particle.
Present invention also offers a kind of preparation method of molybdenum disulfide composite nano-gold photochemical catalyst, comprise the following steps：
1) spherical molybdenum disulfide nano particle is prepared using chemical synthesis；
2) weigh step 1) prepared by nanometer MOS 2 particle be scattered in deionized water and the mixing of absolute ethyl alcohol is molten
In liquid, silane coupler is added, stirring draws appropriate HAuCl to well mixed4Solution is simultaneously added dropwise in mixed solution, is mixed
After closing uniformly, add under sodium citrate solution, constant temperature and stir 30-40min, obtain colloid, centrifuge and wash, circulate three times,
Dried in drying box, produce molybdenum disulfide composite nano-gold photochemical catalyst.
Preferably, silane coupler used is KH-550, and nanometer MOS 2 particle and KH-550 amount ratio are 1:
80g/mL。
Preferably, deionized water and the consumption volume ratio of absolute ethyl alcohol are (3-5)：1.
Preferably, nanometer MOS 2 particle and deionized water and the amount ratio 1 of the mixed solution of absolute ethyl alcohol:(800-
1000)g/mL。
Preferably, HAuCl used4The concentration of solution is 0.005-0.01mol/L, nanometer MOS 2 particle and HAuCl4
The amount ratio of solution is 1：(400-800)g/mL.
Preferably, the concentration of sodium citrate solution used is 0.1-0.15mol/L, nanometer MOS 2 particle and citric acid
The amount ratio of sodium solution is 1:(800-1000)g/mL.
Preferably, add sodium citrate solution to stir after constant temperature at 80-95 DEG C, the drying temperature of drying box is 80-95
DEG C, drying time is 7-8h.
Preferably, in step 1) in, spherical curing is prepared using thioacetamide and sodium molybdate using chemical synthesis
Molybdenum nano particle, concrete mode is as follows：
Compare 2 according to weight is weighed:1 thioacetamide and sodium molybdate, gained mixture are added in deionized water, heating is stirred
Mix, the thioacetamide of addition and the mixture of sodium molybdate and the amount ratio of deionized water are 1.5:50g/mL, then adds 1/8
The absolute ethyl alcohol of times deionized water used in volume, adds the concentrated hydrochloric acid of absolute ethyl alcohol used in 1.5 times of volumes, is made after being sufficiently stirred for
Obtain spherical MoS2Presoma sediment；Continue after heating stirring, 10min, carry out filtration washing, dry overnight, by above-mentioned MoS2Before
Drive body sediment and taking-up after 3h is dried at 105 DEG C, under nitrogen protection, sintering soak 50min under the conditions of 480 DEG C drops naturally
Warm to room temperature, be ground after taking-up, obtain spherical MoS2Nano particle.
The present invention has the advantages that：
The invention provides a kind of molybdenum disulfide composite nano-gold photochemical catalyst and preparation method thereof, prepared curing
Molybdenum composite nano-gold photochemical catalyst, is that obtained on spherical molybdenum disulfide nano particle compound is uniformly compounded in by gold nano grain
Photochemical catalyst.The present invention has prepared molybdenum disulfide composite nano-gold photochemical catalyst using sol-gel process, particularly silane
Coupling agent KH-550 is dressing agent, nanometer Au is entrained in into spherical molybdenum disulfide Nanosurface with sol-gel process so that Au receives
Avtive spot increase between rice corpuscles and molybdenum disulfide, so that the catalytic performance after molybdenum disulfide doping Au is improved.
Embodiment
The embodiment of the present invention provides a kind of molybdenum disulfide composite nano-gold photochemical catalyst, is uniformly combined by gold nano grain
The composite photo-catalyst obtained on spherical molybdenum disulfide nano particle.
Technical scheme is clearly and completely described below in conjunction with embodiment, it is clear that described reality
It is only a part of embodiment of the invention to apply example, rather than whole embodiments.Based on the embodiment in the present invention, this area is general
The every other embodiment that logical technical staff is obtained under the premise of creative work is not made, belongs to what the present invention was protected
Scope.
A kind of preparation method of molybdenum disulfide composite nano-gold photochemical catalyst provided in an embodiment of the present invention, its feature exists
In comprising the following steps：
1) spherical molybdenum disulfide nano particle is prepared using chemical synthesis；
2) weigh step 1) prepared by nanometer MOS 2 particle be scattered in deionized water and the mixing of absolute ethyl alcohol is molten
In liquid, silane coupler is added, stirring draws appropriate HAuCl to well mixed4Solution is simultaneously added dropwise in mixed solution, is mixed
After closing uniformly, add under sodium citrate solution, constant temperature and stir 30-40min, obtain colloid, centrifuge and wash, circulate three times,
Dried in drying box, produce molybdenum disulfide composite nano-gold photochemical catalyst.
In embodiments of the present invention, silane coupler used is KH-550, nanometer MOS 2 particle and KH-550 use
Amount is than being 1:80g/mL.
In embodiments of the present invention, deionized water and the consumption volume ratio of absolute ethyl alcohol are (3-5)：1.
In embodiments of the present invention, nanometer MOS 2 particle and deionized water and the consumption of the mixed solution of absolute ethyl alcohol
Than 1:(800-1000)g/mL.
In embodiments of the present invention, HAuCl used4The concentration of solution is 0.005-0.01mol/L, molybdenum disulfide nano
Grain and HAuCl4The amount ratio of solution is 1：(400-800)g/mL.
In embodiments of the present invention, the concentration of sodium citrate solution used is 0.1-0.15mol/L, molybdenum disulfide nano
The amount ratio of grain and sodium citrate solution is 1:(800-1000)g/mL.
In embodiments of the present invention, add sodium citrate solution to stir after constant temperature at 80-95 DEG C, drying for drying box is warm
Spend for 80-95 DEG C, drying time is 7-8h.
In embodiments of the present invention, in step 1) in, prepared using chemical synthesis using thioacetamide and sodium molybdate
Spherical molybdenum disulfide nano particle, concrete mode is as follows：
Compare 2 according to weight is weighed:1 thioacetamide and sodium molybdate, gained mixture are added in deionized water, heating is stirred
Mix, the thioacetamide of addition and the mixture of sodium molybdate and the amount ratio of deionized water are 1.5:50g/mL, then adds 1/8
The absolute ethyl alcohol of times deionized water used in volume, adds the concentrated hydrochloric acid of absolute ethyl alcohol used in 1.5 times of volumes, is made after being sufficiently stirred for
Obtain spherical MoS2Presoma sediment；Continue after heating stirring, 10min, carry out filtration washing, dry overnight, by above-mentioned MoS2Before
Drive body sediment and taking-up after 3h is dried at 105 DEG C, under nitrogen protection, sintering soak 50min under the conditions of 480 DEG C drops naturally
Warm to room temperature, be ground after taking-up, obtain spherical MoS2Nano particle.
MoS is carried out using above-mentioned chemical synthesis2The preparation of nano particle, can reduce calcining heat, obtained spherical
MoS2The size of nano particle is 50-100nm, the spherical MoS of acquisition2Nano particle is main by MoS2The part envelope that lamella is constituted
Structure is closed, in obtained MoS2There are many crystal defects in grain edges, beneficial to the enrichment of nanogold particle.
In embodiments of the present invention, KH-550 used can also make dispersant in addition to having coupled action, and adding KH-550 can subtract
Few particle aggregation, makes particle be uniformly dispersed.During reaction, the Au in solution is first with Au3+In the presence of Au3+Gradually with MoS2Surface is connected,
Form Au3/MoS2.The reproducibility of sodium citrate is by Au3Reduction, that is, form Au-MoS2Nano material.Wherein, sodium citrate is not only
Play reduction, moreover it is possible to make system more stable.By the preparation method of the present invention, final acquisition particle is more uniform, pattern is preferable
Target product.Au-MoS prepared by the embodiment of the present invention2Nano material, Au nano-particles sizes are in 5.5-8.5nm scopes
It is interior, MoS2Crystal formation is good, and particle is uniform, soilless sticking phenomenon is produced, Au and MoS2The ratio of doping is more uniform.
It is prepared the embodiments of the invention provide a kind of molybdenum disulfide composite nano-gold photochemical catalyst and preparation method thereof
Molybdenum disulfide composite nano-gold photochemical catalyst, is uniformly to be compounded on spherical molybdenum disulfide nano particle to obtain by gold nano grain
Composite photo-catalyst.The present invention has prepared molybdenum disulfide composite nano-gold photochemical catalyst using sol-gel process, specifically
It is that silane resin acceptor kh-550 is dressing agent, nanometer Au is entrained in spherical molybdenum disulfide Nanosurface with sol-gel process, made
The avtive spot increase between Au nano-particles and molybdenum disulfide is obtained, so that the catalytic performance after molybdenum disulfide doping Au is carried
It is high.
It is further described with reference to specific embodiment.
Embodiment 1
A kind of preparation method of molybdenum disulfide composite nano-gold photochemical catalyst, comprises the following steps：
Step 1, spherical molybdenum disulfide nano particle, mistake using thioacetamide and sodium molybdate prepared using chemical synthesis
Journey is as follows：
1.0gTAA and 0.5g sodium molybdates are weighed in 100mL three-neck flask, then add 50mL's to gained mixture
In deionized water, heating stirring adds 7.5mL absolute ethyl alcohol, adds 11.25mL concentrated hydrochloric acid, is made after being sufficiently stirred for
Spherical MoS2Presoma sediment；Continue after heating stirring, 10min, carry out filtration washing, dry overnight, by above-mentioned MoS2Forerunner
Body sediment is dried after 3h at 105 DEG C and taken out, under nitrogen protection, sintering soak 50min, Temperature fall under the conditions of 480 DEG C
To room temperature, it is ground after taking-up, obtains spherical MoS2Nano particle.
Step 2, the nanometer MOS 2 particle 0.05g weighed prepared by step 1 are scattered in 40mL deionized waters and 10mL
In the mixed solution of absolute ethyl alcohol, 4mL KH-550 is added, stirring uses pipette, extract 20mL to well mixed
0.01mol/L HAuCl4Solution is simultaneously added dropwise in mixed solution, after being well mixed, adds 50mL 0.15mol/L lemon
30min is stirred under acid sodium solution, constant temperature, colloid is obtained, centrifuges and washes, circulates three times, 7h is dried in 90 DEG C of drying boxes, i.e.,
Obtain molybdenum disulfide composite nano-gold photochemical catalyst.
Embodiment 2
A kind of preparation method of molybdenum disulfide composite nano-gold photochemical catalyst, comprises the following steps：
Step 1, spherical molybdenum disulfide nano particle, mistake using thioacetamide and sodium molybdate prepared using chemical synthesis
Journey is as follows：
1.0gTAA and 0.5g sodium molybdates are weighed in 100mL three-neck flask, then add 50mL's to gained mixture
In deionized water, heating stirring adds 7.5mL absolute ethyl alcohol, adds 11.25mL concentrated hydrochloric acid, is made after being sufficiently stirred for
Spherical MoS2Presoma sediment；Continue after heating stirring, 10min, carry out filtration washing, dry overnight, by above-mentioned MoS2Forerunner
Body sediment is dried after 3h at 105 DEG C and taken out, under nitrogen protection, sintering soak 50min, Temperature fall under the conditions of 480 DEG C
To room temperature, it is ground after taking-up, obtains spherical MoS2Nano particle.
Step 2, the nanometer MOS 2 particle 0.05g weighed prepared by step 1 are scattered in 30mL deionized waters and 10mL
In the mixed solution of absolute ethyl alcohol, 4mL KH-550 is added, stirring uses pipette, extract 40mL to well mixed
0.005mol/L HAuCl4Solution is simultaneously added dropwise in mixed solution, after being well mixed, adds 40mL 0.15mol/L lemon
30min is stirred under lemon acid sodium solution, constant temperature, colloid is obtained, centrifuges and washes, circulates three times, 7h is dried in 95 DEG C of drying boxes,
Produce molybdenum disulfide composite nano-gold photochemical catalyst.
Embodiment 3
A kind of preparation method of molybdenum disulfide composite nano-gold photochemical catalyst, comprises the following steps：
Step 1, spherical molybdenum disulfide nano particle, mistake using thioacetamide and sodium molybdate prepared using chemical synthesis
Journey is as follows：
1.0gTAA and 0.5g sodium molybdates are weighed in 100mL three-neck flask, then add 50mL's to gained mixture
In deionized water, heating stirring adds 7.5mL absolute ethyl alcohol, adds 11.25mL concentrated hydrochloric acid, is made after being sufficiently stirred for
Spherical MoS2Presoma sediment；Continue after heating stirring, 10min, carry out filtration washing, dry overnight, by above-mentioned MoS2Forerunner
Body sediment is dried after 3h at 105 DEG C and taken out, under nitrogen protection, sintering soak 50min, Temperature fall under the conditions of 480 DEG C
To room temperature, it is ground after taking-up, obtains spherical MoS2Nano particle.
Step 2, the nanometer MOS 2 particle 0.05g weighed prepared by step 1 be scattered in 40mL deionized waters and 8mL without
In the mixed solution of water-ethanol, 4mL KH-550 is added, stirring uses pipette, extract 30mL to well mixed
0.008mol/L HAuCl4Solution is simultaneously added dropwise in mixed solution, after being well mixed, adds 45mL 0.12mol/L lemon
30min is stirred under lemon acid sodium solution, constant temperature, colloid is obtained, centrifuges and washes, circulates three times, 8h is dried in 80 DEG C of drying boxes,
Produce molybdenum disulfide composite nano-gold photochemical catalyst.
, but those skilled in the art once know basic creation although preferred embodiments of the present invention have been described
Property concept, then can make other change and modification to these embodiments.So, appended claims are intended to be construed to include excellent
Select embodiment and fall into having altered and changing for the scope of the invention.
Obviously, those skilled in the art can carry out the essence of various changes and modification without departing from the present invention to the present invention
God and scope.So, if these modifications and variations of the present invention belong to the scope of the claims in the present invention and its equivalent technologies
Within, then the present invention is also intended to comprising including these changes and modification.
Claims (9)
1. a kind of molybdenum disulfide composite nano-gold photochemical catalyst, it is characterised in that be uniformly be compounded in by gold nano grain it is spherical
The composite photo-catalyst obtained on nanometer MOS 2 particle.
2. a kind of preparation method of molybdenum disulfide composite nano-gold photochemical catalyst, it is characterised in that comprise the following steps：
1) spherical molybdenum disulfide nano particle is prepared using chemical synthesis；
2) weigh step 1) prepared by nanometer MOS 2 particle be scattered in the mixed solution of deionized water and absolute ethyl alcohol,
Silane coupler is added, stirring draws appropriate HAuCl to well mixed4Solution is simultaneously added dropwise in mixed solution, is well mixed
Afterwards, add under sodium citrate solution, constant temperature and stir 30-40min, obtain colloid, centrifuge and wash, circulate three times, in drying
Dried in case, produce molybdenum disulfide composite nano-gold photochemical catalyst.
3. preparation method as claimed in claim 2, it is characterised in that silane coupler used is KH-550, molybdenum disulfide is received
Rice grain and KH-550 amount ratio are 1:80g/mL.
4. preparation method as claimed in claim 2, it is characterised in that deionized water and the consumption volume ratio of absolute ethyl alcohol are
(3-5)：1.
5. preparation method as claimed in claim 2, it is characterised in that nanometer MOS 2 particle and deionized water and anhydrous second
The amount ratio 1 of the mixed solution of alcohol:(800-1000)g/mL.
6. preparation method as claimed in claim 2, it is characterised in that HAuCl used4The concentration of solution is 0.005-
0.01mol/L, nanometer MOS 2 particle and HAuCl4The amount ratio of solution is 1：(400-800)g/mL.
7. preparation method as claimed in claim 2, it is characterised in that the concentration of sodium citrate solution used is 0.1-
The amount ratio of 0.15mol/L, nanometer MOS 2 particle and sodium citrate solution is 1:(800-1000)g/mL.
8. preparation method as claimed in claim 2, it is characterised in that add sodium citrate solution after constant temperature at 80-95 DEG C
Stirring, the drying temperature of drying box is 80-95 DEG C, and drying time is 7-8h.
9. preparation method as claimed in claim 2, it is characterised in that in step 1) in, utilize thio using chemical synthesis
Acetamide and sodium molybdate prepare spherical molybdenum disulfide nano particle, and concrete mode is as follows：
Compare 2 according to weight is weighed:1 thioacetamide and sodium molybdate, gained mixture are added in deionized water, heating stirring,
The thioacetamide of addition and the mixture of sodium molybdate and the amount ratio of deionized water are 1.5:50g/mL, then adds 1/8 times
The absolute ethyl alcohol of deionized water used in volume, adds the concentrated hydrochloric acid of absolute ethyl alcohol used in 1.5 times of volumes, is made after being sufficiently stirred for
Spherical MoS2Presoma sediment；Continue after heating stirring, 10min, carry out filtration washing, dry overnight, by above-mentioned MoS2Forerunner
Body sediment is dried after 3h at 105 DEG C and taken out, under nitrogen protection, sintering soak 50min, Temperature fall under the conditions of 480 DEG C
To room temperature, it is ground after taking-up, obtains spherical MoS2Nano particle.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1722316A (en) * | 2000-01-17 | 2006-01-18 | 松下电器产业株式会社 | Method for fabricating resistor |
| CN105776335A (en) * | 2014-12-16 | 2016-07-20 | 中国石油天然气股份有限公司 | Preparation method of high-purity phase spherical molybdenum disulfide |
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| CN1722316A (en) * | 2000-01-17 | 2006-01-18 | 松下电器产业株式会社 | Method for fabricating resistor |
| CN105776335A (en) * | 2014-12-16 | 2016-07-20 | 中国石油天然气股份有限公司 | Preparation method of high-purity phase spherical molybdenum disulfide |
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