CN107744818A - Molybdenum disulfide loads the preparation method of silver-colored photochemical catalyst - Google Patents
Molybdenum disulfide loads the preparation method of silver-colored photochemical catalyst Download PDFInfo
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- CN107744818A CN107744818A CN201710990461.1A CN201710990461A CN107744818A CN 107744818 A CN107744818 A CN 107744818A CN 201710990461 A CN201710990461 A CN 201710990461A CN 107744818 A CN107744818 A CN 107744818A
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- Prior art keywords
- molybdenum disulfide
- preparation
- mos
- load silver
- silver
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- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 51
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000003054 catalyst Substances 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 229910052709 silver Inorganic materials 0.000 claims abstract description 19
- 239000004332 silver Substances 0.000 claims abstract description 19
- 229910052961 molybdenite Inorganic materials 0.000 claims description 17
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000000725 suspension Substances 0.000 claims description 9
- 238000001291 vacuum drying Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 6
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 3
- 238000002372 labelling Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 238000003760 magnetic stirring Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000001556 precipitation Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 238000010992 reflux Methods 0.000 claims description 3
- 230000004044 response Effects 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 235000015393 sodium molybdate Nutrition 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical class CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 17
- 238000007146 photocatalysis Methods 0.000 abstract description 15
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 14
- 239000001257 hydrogen Substances 0.000 abstract description 14
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 14
- 239000000463 material Substances 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000000034 method Methods 0.000 abstract description 6
- 239000002114 nanocomposite Substances 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 2
- 230000002194 synthesizing effect Effects 0.000 abstract description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 13
- 239000000047 product Substances 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- -1 transition metal sulfide Chemical class 0.000 description 1
Classifications
-
- B01J35/39—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
Abstract
The invention discloses a kind of method for preparing catalyst of molybdenum disulfide load silver, mainly comprises the following steps molybdenum disulfide and prepares the preparation that silver is loaded with molybdenum disulfide.The purpose is to by providing molybdenum disulfide load silver, a kind of nano composite material with stronger photocatalysis performance has been made, its photocatalysis hydrogen production performance activity is greatly improved, and nano composite material has environmental-protecting performance, synthesizing and environment will not both polluted in photocatalytic process, user will not also damaged.
Description
Technical field
The present invention relates to the photochemical catalyst preparation method of molybdenum disulfide load silver, belong to catalysis material technical field.
Background technology
Molybdenum disulfide is a kind of typical stratiform transition metal sulfide, has similar structure with graphene, turns in light
Change, each field such as photocatalysis has been widely used, to producing with before great for degradable organic pollutant and energy hydrogen
Scape.Molybdenum disulfide nano sheet has " sandwich " structure by what the individual layer or multilayer molybdenum disulfide of hexagonal crystal system formed
Two dimensional crystal material.
There is weaker Van der Waals force in molybdenum disulfide, have good lubricity between layers.The energy band of molybdenum disulfide
Gap is 1.29~1.90eV, gradually widely studied by people in terms of energy hydrogen manufacturing.The chemical property of molybdenum disulfide is very stable, often
The lower presence that can be stable of temperature, is not easy to react with other materials, thus molybdenum disulfide in photocatalysis field with greatly grinding
Study carefully meaning and application potential.Because molybdenum disulfide has the characteristics such as the strong, unsaturation of huge specific surface area, absorption property, institute
To study the utilization of molybdenum disulfide at present and be applicable as one of focus material of people's research.
The content of the invention
The purpose of the present invention is by providing molybdenum disulfide load silver, a kind of receiving with stronger photocatalysis performance being made
Nano composite material, its photocatalysis hydrogen production performance activity is greatly improved, and nano composite material has environmental-protecting performance, is closing
Into with environment will not both be polluted in photocatalytic process, user will not also be damaged.
The technical solution adopted by the present invention is：The preparation method of the photochemical catalyst of molybdenum disulfide load silver, passes through hydro-thermal method
Prepare, it is characterised in that preparation process is as follows：
（1）It is prepared by molybdenum disulfide：0.2419g sodium molybdates and 0.37565g thioacetamides are weighed, is dissolved in 40ml deionization
In water, the solution until being clarified is continuously agitated, then liquid is moved into 50ml reactor, anti-under conditions of 220 DEG C
After answering 24h, question response to terminate, room temperature is naturally cooled to, is centrifuged, separation, precipitation is respectively washed with deionized water and absolute ethyl alcohol respectively
Wash 3 times, 24h is finally dried in vacuo in 80 DEG C of vacuum drying chamber, last Product Labeling is S-MoS2；
（2）The preparation of molybdenum disulfide load silver：Weigh 1g above-mentioned steps obtained S-MoS2It is added to 20mlAgNO3Solution
In, wherein CAgNO3=0.002943427M, ultrasonic 30min, the suspension of black is obtained, 0.1M is used under conditions of stirring is not stopped
NaOH solution regulation suspension pH=8-9, it is then subjected to cooling for reflux under 75 DEG C of oil bath pans and magnetic stirring apparatus,
Reaction time is 5h, after suspension naturally cools to room temperature, respectively with respectively washing 3 times of deionized water and absolute ethyl alcohol, then
Product is subjected to vacuum drying 48h in 80 DEG C of vacuum drying chamber, is in nitrogen protection and temperature by dry product finally
Under conditions of 300 DEG C, the tube furnace for being 2 DEG C/min in calcining heating rate carries out calcining 1h, and molybdenum disulfide load silver is made
Catalyst, labeled as Ag-S-MoS2。
The catalyst that the present invention prepares molybdenum disulfide load silver has stronger photocatalysis Hydrogen Evolution Performance.By hydro-thermal method and forge
Burning method, Ag-S-MoS2 compounds are made, this compound expands the absorption model to ultraviolet-visible in photocatalytic process
Enclose, strengthen the absorption to light, improve the photocatalysis Hydrogen Evolution Performance of product；Ag-S-MoS2Compound is in photocatalysis liberation of hydrogen
In circulation experiment, it can be recycled for multiple times.
Advantages of the present invention：1st, the catalyst of molybdenum disulfide load silver has very strong photocatalysis Hydrogen Evolution Performance, and itself
Possess good environmental-protecting performance, synthesizing and both environment will not have been polluted in photocatalytic process, user will not also be made
Into any injury.2、S-MoS2Photocatalysis hydrogen production speed be 0.887mmolg-1h-1, Ag-S-MoS2Photocatalysis hydrogen production speed
For 1.247mmolg-1h-1, by S-MoS2And Ag-S-MoS2The comparison of photocatalysis hydrogen production, the curing of load silver is drawn
The photocatalysis Hydrogen Evolution Performance of molybdenum is improved.3rd, obtained Ag-S-MoS2Compound is bigger than the surface area of monomer molybdenum disulfide,
More avtive spot sulphur atoms can be provided for photocatalysis liberation of hydrogen.4th, the catalyst prod of this molybdenum disulfide load silver produces it
It is prepared by preceding nobody.
Brief description of the drawings
Fig. 1 is the catalyst Hydrogen Evolution Performance figure of molybdenum disulfide of the present invention load silver.
Fig. 2 is the catalyst transmission plot of molybdenum disulfide of the present invention load silver, is schemed（a）For S-MoS2, figure（b）For Ag-S-
MoS2。
Embodiment
Embodiment 1
It is prepared by molybdenum disulfide：
0.2419g sodium molybdates and 0.37565g thioacetamides are weighed, is dissolved in 40ml deionized water, is continuously agitated straight
To the solution clarified, then in liquid immigration 50ml reactor, 24h is reacted under conditions of 220 DEG C, question response terminates
Afterwards, room temperature is naturally cooled to, is centrifuged, separation, precipitation uses respectively washing 3 times of deionized water and absolute ethyl alcohol respectively, finally at 80 DEG C
Vacuum drying chamber in be dried in vacuo 24h, last Product Labeling is S-MoS2；
Embodiment 2
The preparation of molybdenum disulfide load silver：
Weigh 1g above-mentioned steps obtained S-MoS2It is added in 20mlAgNO3 solution, wherein（CAgNO3=
0.002943427M）, ultrasonic 30min, the suspension of black is obtained, is adjusted under conditions of stirring is not stopped with 0.1M NaOH solution
PH=8-9 of suspension is saved, then it carries out to cooling for reflux under 75 DEG C of oil bath pans and magnetic stirring apparatus, reaction time 5h,
After suspension naturally cools to room temperature, respectively washed 3 times with deionized water and absolute ethyl alcohol respectively, then by product at 80 DEG C
Vacuum drying 48h is carried out in vacuum drying chamber, is under conditions of 300 DEG C in nitrogen protection and temperature by dry product finally,
The tube furnace for being 2 DEG C/min in calcining heating rate carries out calcining 1h, and the catalyst of molybdenum disulfide load silver is made, is labeled as
Ag-S-MoS2。
Claims (1)
1. the preparation method of the photochemical catalyst of molybdenum disulfide load silver, is prepared, it is characterised in that preparation process is such as by hydro-thermal method
Under：
It is prepared by the first step, molybdenum disulfide：
（1）0.2419g sodium molybdates and 0.37565g thioacetamides are weighed, is dissolved in 40ml deionized water, is ceaselessly stirred
Mix the solution until being clarified；
（2）Then liquid is moved into 50ml reactor, and 24h, after question response terminates, natural cooling are reacted under conditions of 220 DEG C
To room temperature, centrifuge, separation, precipitation is respectively with respectively washing 3 times of deionized water and absolute ethyl alcohol；
（3）24h is finally dried in vacuo in 80 DEG C of vacuum drying chamber, last Product Labeling is S-MoS2；
Second step, the preparation of molybdenum disulfide load silver：
（1）Weigh 1g above-mentioned steps obtained S-MoS2It is added to 20mlAgNO3In solution, wherein CAgNO3=
0.002943427M, ultrasonic 30min, the suspension of black is obtained, adjusted under conditions of stirring is not stopped with 0.1M NaOH solution
Save pH=8-9 of suspension；
（2）Then it is carried out to cooling for reflux under 75 DEG C of oil bath pans and magnetic stirring apparatus, reaction time 5h, treat suspension certainly
After being so cooled to room temperature, respectively washed 3 times with deionized water and absolute ethyl alcohol respectively, then by vacuum drying chamber of the product at 80 DEG C
In carry out vacuum drying 48h；
（3）Be under conditions of 300 DEG C in nitrogen protection and temperature by dry product finally, calcining heating rate be 2 DEG C/
Min tube furnace carries out calcining 1h, the catalyst of molybdenum disulfide load silver is made, labeled as Ag-S-MoS2。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710990461.1A CN107744818A (en) | 2017-10-23 | 2017-10-23 | Molybdenum disulfide loads the preparation method of silver-colored photochemical catalyst |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710990461.1A CN107744818A (en) | 2017-10-23 | 2017-10-23 | Molybdenum disulfide loads the preparation method of silver-colored photochemical catalyst |
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|---|---|
| CN107744818A true CN107744818A (en) | 2018-03-02 |
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|---|---|---|---|
| CN201710990461.1A Pending CN107744818A (en) | 2017-10-23 | 2017-10-23 | Molybdenum disulfide loads the preparation method of silver-colored photochemical catalyst |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108745380A (en) * | 2018-06-28 | 2018-11-06 | 合肥工业大学 | A kind of preparation method carrying silver-colored molybdenum disulfide nano tube composite electro catalytic liberation of hydrogen material |
| CN109622044A (en) * | 2018-12-19 | 2019-04-16 | 郑州大学 | A kind of efficient liberation of hydrogen catalyst material, preparation method and application |
| CN110560093A (en) * | 2019-09-16 | 2019-12-13 | 南昌航空大学 | Two-dimensional MoS2Preparation method of Cu-loaded photocatalyst |
| CN110583691A (en) * | 2019-09-19 | 2019-12-20 | 南京工业大学 | Reductive graphene oxide-molybdenum disulfide-silver ternary composite antibacterial material and preparation method and application thereof |
| CN114887060A (en) * | 2022-05-24 | 2022-08-12 | 南京师范大学 | Near-infrared carbon dot/molybdenum disulfide composite material and application thereof |
| CN116440927A (en) * | 2023-04-25 | 2023-07-18 | 景德镇陶瓷大学 | Preparation method of silver-modified molybdenum sulfide nanoflower |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108745380A (en) * | 2018-06-28 | 2018-11-06 | 合肥工业大学 | A kind of preparation method carrying silver-colored molybdenum disulfide nano tube composite electro catalytic liberation of hydrogen material |
| CN109622044A (en) * | 2018-12-19 | 2019-04-16 | 郑州大学 | A kind of efficient liberation of hydrogen catalyst material, preparation method and application |
| CN110560093A (en) * | 2019-09-16 | 2019-12-13 | 南昌航空大学 | Two-dimensional MoS2Preparation method of Cu-loaded photocatalyst |
| CN110560093B (en) * | 2019-09-16 | 2021-11-19 | 南昌航空大学 | Two-dimensional MoS2Preparation method of Cu-loaded photocatalyst |
| CN110583691A (en) * | 2019-09-19 | 2019-12-20 | 南京工业大学 | Reductive graphene oxide-molybdenum disulfide-silver ternary composite antibacterial material and preparation method and application thereof |
| CN114887060A (en) * | 2022-05-24 | 2022-08-12 | 南京师范大学 | Near-infrared carbon dot/molybdenum disulfide composite material and application thereof |
| CN116440927A (en) * | 2023-04-25 | 2023-07-18 | 景德镇陶瓷大学 | Preparation method of silver-modified molybdenum sulfide nanoflower |
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Application publication date: 20180302 |