CN105536684A - Preparation method of molybdenum disulfide-silver sulfide composite nano-grade adsorption-photocatalyst - Google Patents
Preparation method of molybdenum disulfide-silver sulfide composite nano-grade adsorption-photocatalyst Download PDFInfo
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- CN105536684A CN105536684A CN201510975749.2A CN201510975749A CN105536684A CN 105536684 A CN105536684 A CN 105536684A CN 201510975749 A CN201510975749 A CN 201510975749A CN 105536684 A CN105536684 A CN 105536684A
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0218—Compounds of Cr, Mo, W
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0233—Compounds of Cu, Ag, Au
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0262—Compounds of O, S, Se, Te
- B01J20/0266—Compounds of S
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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
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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
Abstract
The invention provides a preparation method of a molybdenum disulfide-silver sulfide composite nano-grade adsorption-photocatalyst. According to the invention, (NH4)2MoO4, KSCN and NH2OH.HCl are adopted as raw material for synthesizing molybdenum disulfide nanoflowers with a hydrothermal method; the obtained molybdenum disulfide nanoflowers and AgNO3 are added into deionized water; stirring is carried out, and an obtained mixture is added into a reaction kettle; the reaction kettle is sealed, and a thermostatic reaction is carried out; and the obtained reaction product is separated, washed and dried, such that the molybdenum disulfide-silver sulfide composite nano-grade adsorption-photocatalyst is obtained. The preparation method provided by the invention has the advantages of low cost, easy and easy-to-control production process, and high product yield. The method is suitable for large-scale industrial productions.
Description
Technical field
The invention belongs to technical field of nano material, be specifically related to the preparation method of a kind of molybdenum bisuphide-silver sulfide composite Nano absorption-photochemical catalyst.
Background technology
Along with the fast development of human industry's civilization; the problem of environmental pollution brought is on the rise; problem of environmental pollution becomes a large problem directly threatening the needs of human survival anxious to be resolved, and thus environmental protection and sustainable development become the matter of utmost importance that people must consider.Within 1972, Fujishjma and Honda has delivered about TiO on Nature magazine
2the paper of electrode glazing decomposition water, can be regarded as the mark that a multiphase photocatalysis New Times starts.But, TiO
2visible ray utilization rate lower, what therefore hold it back further develops, and therefore, the importance of the visible light catalyst of Development of Novel is self-evident.
Silver sulfide can carrying semiconductor material as high narrow of a kind of chemical stability of IV-V race, has been widely used in the manufacturing industry such as photocell photoconductive device, infrared detector, fast-ionic conductor.The comparatively Large ratio surface that silver sulfide nanometer particles is formed due to it and produce significant quantum size effect, makes it in light absorption and sensing, catalysis and photoelectricity etc., show the property different from body phase material.Patent CN103785848A discloses a kind of method of single tank synthesis Ag-silver sulfide/CdS heterojunction structure, its objective is that the synthesis by this three-system photochemical catalyst improves the photocatalysis performance of silver sulfide further.Molybdenum bisuphide, due to the structure of its uniqueness, is widely used in the field such as lubrication, lithium electricity, ultracapacitor, and research in recent years shows also to show very excellent performance at absorption, photocatalysis field molybdenum bisuphide.The molybdenum bisuphide with nanostructured is had been further upgraded in many performances, show the following aspects highlightedly: specific area is very big, adsorption capacity is stronger, reactivity is high, the performance of catalytic performance especially catalytic hydrogenation desulfurization is stronger, can be used to prepare special catalysis material and gas storing material.Therefore, the synthesis of molybdenum bisuphide-silver sulfide functional composite nano material, contributes to the photo-catalysis capability strengthening photochemical catalyst, makes it have very outstanding absorption property simultaneously; In addition the fields such as air-sensitive, electrochemistry and lithium electricity can also be applied to.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art and the preparation method providing a kind of molybdenum bisuphide-silver sulfide composite Nano absorption-photochemical catalyst, the method is with low cost, technique is simple, and productive rate is high.
The preparation method of molybdenum bisuphide-silver sulfide composite Nano absorption-photochemical catalyst, comprises the following steps:
Step 1, with (NH
4)
2moO
4, KSCN and NH
2oHHCl is raw water thermal synthesis molybdenum disulfide nano flower;
Step 2, by step 1 gained molybdenum disulfide nano flower and AgNO
3add in deionized water, stir, move into reactor, sealing, after isothermal reaction, obtains product;
Step 3, is separated step 2 gained product, and washing, drying, obtain molybdenum bisuphide-silver sulfide composite Nano absorption-photochemical catalyst.
Further, in step 1, the temperature of Hydrothermal Synthesis is 150 ~ 500 DEG C, and the time is 16 ~ 48h.
Further, Mo and AgNO that in step 2, molybdenum disulfide nano is spent
3ag mol ratio be 1:1 ~ 8.
Further, the temperature of isothermal reaction in step 2 is 90 DEG C ~ 260 DEG C, and the time is 12 ~ 36h.
Preparation method's cost of the present invention is inexpensive, and production technology is simple and easy to control, and efficiency of pcr product is high, is applicable to large-scale industrial production; Gained molybdenum bisuphide-silver sulfide composite Nano absorption-photochemical catalyst not only has excellent photocatalysis performance, also has good absorption property simultaneously.
Accompanying drawing explanation
Fig. 1 is the XRD spectra of the molybdenum bisuphide-silver sulfide composite Nano absorption-photochemical catalyst of embodiment 1;
Fig. 2 is the SEM figure of the molybdenum bisuphide-silver sulfide composite Nano absorption-photochemical catalyst of embodiment 1;
Fig. 3 is the photocatalysis curve map of the molybdenum bisuphide-silver sulfide composite Nano absorption-photochemical catalyst of embodiment 1;
Fig. 4 is the adsorption curve figure of the molybdenum bisuphide-silver sulfide composite Nano absorption-photochemical catalyst of embodiment 1.
Detailed description of the invention
The present invention is further described below by way of detailed description of the invention, as known by the technical knowledge, the present invention also describes by other the scheme not departing from the technology of the present invention feature, and the change therefore within the scope of the present invention all or equivalent scope of the invention is all included in the invention.
Embodiment 1
By 0.24g (NH
4)
2moO
4, 0.32gKSCN and 0.28gNH
2oHHCl is dissolved in the deionized water of 60mL, after dissolving completely, continues to stir 30min, then is transferred in the stainless steel cauldron of 100mL by mixed liquor, is placed in vacuum drying chamber in 180 DEG C of insulation 24h, is cooled to room temperature.Product, after centrifugation, uses deionized water and absolute ethyl alcohol cyclic washing respectively, and finally 80 DEG C of dry 10h obtain the powder product of grey black under vacuum, i.e. molybdenum disulfide nano flower.
By 0.85gAgNO
3be distributed in the deionized water of 60mL with 0.16g molybdenum bisuphide, after Keep agitation 30min, then mixed liquor be transferred in the stainless steel cauldron of 100mL, be placed in vacuum drying chamber in 160 DEG C of insulation 24h, be cooled to room temperature.Product, after centrifugation, uses deionized water and absolute ethyl alcohol cyclic washing respectively, and finally 80 DEG C of dry 10h obtain the product powder of black under vacuum, i.e. molybdenum bisuphide-silver sulfide composite Nano absorption-photochemical catalyst.
In Fig. 1, a, b, c are the XRD figure of molybdenum bisuphide, molybdenum bisuphide-silver sulfide, silver sulfide respectively, and peaks all in b can be well corresponding with pure silver sulfide crystal face and molybdenum bisuphide crystal face, illustrates that synthetic product is molybdenum bisuphide-silver sulfide.Fig. 2 is the SEM figure of product, and can find out clearly from figure, flower-shaped molybdenum bisuphide loads to the surface of particle silver sulfide, defines molybdenum bisuphide-silver sulfide heterojunction structure.Fig. 3 is the photocatalysis of photochemical catalyst to rhodamine B, Fig. 4 is the absorption figure of photochemical catalyst to rhodamine B, as can be seen from the figure molybdenum bisuphide-silver sulfide heterojunction structure has excellent photocatalysis performance, and in 90min, 100% degrades 10g/L rhodamine B, also has good absorption property simultaneously.
Embodiment 2
By 0.24g (NH
4)
2moO
4, 0.32gKSCN and 0.28gNH
2oHHCl is dissolved in the deionized water of 60mL, after dissolving completely, continues to stir 30min, then is transferred in the stainless steel cauldron of 100mL by mixed liquor, is placed in vacuum drying chamber in 180 DEG C of insulation 24h, is cooled to room temperature.Product, after centrifugation, uses deionized water and absolute ethyl alcohol cyclic washing respectively, and finally 80 DEG C of dry 10h obtain the powder product of grey black under vacuum, i.e. molybdenum disulfide nano flower.
By 0.17gAgNO
3be distributed in the deionized water of 60mL with 0.16g molybdenum bisuphide, after Keep agitation 30min, then mixed liquor be transferred in the stainless steel cauldron of 100mL, be placed in vacuum drying chamber in 160 DEG C of insulation 24h, be cooled to room temperature.Product, after centrifugation, uses deionized water and absolute ethyl alcohol cyclic washing respectively, and finally 80 DEG C of dry 10h obtain the product powder of black under vacuum, i.e. molybdenum bisuphide-silver sulfide composite Nano absorption-photochemical catalyst.
Can see that flower-shaped molybdenum bisuphide loads to the surface of particle silver sulfide in the SEM figure of products therefrom molybdenum bisuphide-silver sulfide composite Nano absorption-photochemical catalyst, define molybdenum bisuphide-silver sulfide heterojunction structure; Products therefrom not only has excellent photocatalysis performance, also has good absorption property simultaneously.
Embodiment 3
By 0.24g (NH
4)
2moO
4, 0.32gKSCN and 0.28gNH
2oHHCl is dissolved in the deionized water of 60mL, after dissolving completely, continues to stir 30min, then is transferred in the stainless steel cauldron of 100mL by mixed liquor, is placed in vacuum drying chamber in 320 DEG C of insulation 18h, is cooled to room temperature.Product, after centrifugation, uses deionized water and absolute ethyl alcohol cyclic washing respectively, and finally 80 DEG C of dry 10h obtain the powder product of grey black under vacuum, i.e. molybdenum disulfide nano flower.
By 0.54gAgNO
3be distributed in the deionized water of 60mL with 0.16g molybdenum bisuphide, after Keep agitation 30min, then mixed liquor be transferred in the stainless steel cauldron of 100mL, be placed in vacuum drying chamber in 120 DEG C of insulation 24h, be cooled to room temperature.Product, after centrifugation, uses deionized water and absolute ethyl alcohol cyclic washing respectively, and finally 80 DEG C of dry 10h obtain the product powder of black under vacuum, i.e. molybdenum bisuphide-silver sulfide composite Nano absorption-photochemical catalyst.
Can see that flower-shaped molybdenum bisuphide loads to the surface of particle silver sulfide in the SEM figure of products therefrom molybdenum bisuphide-silver sulfide composite Nano absorption-photochemical catalyst, define molybdenum bisuphide-silver sulfide heterojunction structure; Products therefrom not only has excellent photocatalysis performance, also has good absorption property simultaneously.
Claims (5)
1. the preparation method of molybdenum bisuphide-silver sulfide composite Nano absorption-photochemical catalyst, is characterized in that: comprise the following steps:
Step 1 is raw water thermal synthesis molybdenum disulfide nano flower with (NH4) 2MoO4, KSCN and NH2OHHCl;
Step 2, by step 1 gained molybdenum disulfide nano flower and AgNO
3add in deionized water, stir, move into reactor, sealing, after isothermal reaction, obtains product;
Step 3, is separated step 2 gained product, and washing, drying, obtain molybdenum bisuphide-silver sulfide composite Nano absorption-photochemical catalyst.
2. the preparation method of molybdenum bisuphide according to claim 1-silver sulfide composite Nano absorption-photochemical catalyst, is characterized in that: in step 1, the temperature of Hydrothermal Synthesis is 150 ~ 500 DEG C, and the time is 16 ~ 48h.
3. the preparation method of molybdenum bisuphide according to claim 1-silver sulfide composite Nano absorption-photochemical catalyst, is characterized in that: Mo and AgNO of molybdenum disulfide nano flower in step 2
3ag mol ratio be 1:1 ~ 8.
4. the preparation method of molybdenum bisuphide according to claim 1-silver sulfide composite Nano absorption-photochemical catalyst, is characterized in that: the temperature of isothermal reaction in step 2 is 90 DEG C ~ 260 DEG C.
5. the preparation method of molybdenum bisuphide according to claim 1-silver sulfide composite Nano absorption-photochemical catalyst, is characterized in that: the time of isothermal reaction in step 2 is 12 ~ 36h.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106179412A (en) * | 2016-07-26 | 2016-12-07 | 陕西科技大学 | One prepares lamellar SmS CrS2interlayer does not mate the method for compound |
| 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 |
| CN109012711A (en) * | 2018-08-30 | 2018-12-18 | 西京学院 | A method of improving transition metal composite material catalytic performance |
| CN109126828A (en) * | 2018-09-05 | 2019-01-04 | 中国科学院东北地理与农业生态研究所 | Z-type flower ball-shaped molybdenum disulfide/silver sulfide/silver composite photo-catalyst preparation method and applications |
| CN109482201A (en) * | 2018-12-11 | 2019-03-19 | 西安理工大学 | A kind of preparation method of Ag doping molybdenum disulfide nano sheet photochemical catalyst |
| CN109888259A (en) * | 2019-04-08 | 2019-06-14 | 陕西科技大学 | A kind of MoS2Nano combined anode of magnesium ion battery material of@GO and preparation method and application |
| CN113841708A (en) * | 2021-11-08 | 2021-12-28 | 陕西科技大学 | Silver sulfide/molybdenum disulfide/acidified attapulgite nano composite light-driven antibacterial material and preparation method and application thereof |
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| CN103611550A (en) * | 2013-11-21 | 2014-03-05 | 镇江市高等专科学校 | Preparation method of molybdenum disulfide-silver metavanadate composite nano photocatalyst |
| CN104307537A (en) * | 2014-09-22 | 2015-01-28 | 江苏大学 | Preparation method of MoS2 / Ag2S nano-composite photocatalytic material |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106179412A (en) * | 2016-07-26 | 2016-12-07 | 陕西科技大学 | One prepares lamellar SmS CrS2interlayer does not mate the method for compound |
| CN106179412B (en) * | 2016-07-26 | 2018-08-24 | 陕西科技大学 | It is a kind of to prepare sheet SmS-CrS2The method that interlayer mismatches compound |
| 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 |
| CN109012711A (en) * | 2018-08-30 | 2018-12-18 | 西京学院 | A method of improving transition metal composite material catalytic performance |
| CN109126828A (en) * | 2018-09-05 | 2019-01-04 | 中国科学院东北地理与农业生态研究所 | Z-type flower ball-shaped molybdenum disulfide/silver sulfide/silver composite photo-catalyst preparation method and applications |
| CN109126828B (en) * | 2018-09-05 | 2021-07-06 | 中国科学院东北地理与农业生态研究所 | Preparation method and application of Z-shaped flower spherical molybdenum disulfide/silver sulfide/silver composite photocatalyst |
| CN109482201A (en) * | 2018-12-11 | 2019-03-19 | 西安理工大学 | A kind of preparation method of Ag doping molybdenum disulfide nano sheet photochemical catalyst |
| CN109482201B (en) * | 2018-12-11 | 2021-08-06 | 西安理工大学 | Preparation method of silver-doped molybdenum disulfide nanosheet photocatalyst |
| CN109888259A (en) * | 2019-04-08 | 2019-06-14 | 陕西科技大学 | A kind of MoS2Nano combined anode of magnesium ion battery material of@GO and preparation method and application |
| CN113841708A (en) * | 2021-11-08 | 2021-12-28 | 陕西科技大学 | Silver sulfide/molybdenum disulfide/acidified attapulgite nano composite light-driven antibacterial material and preparation method and application thereof |
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Application publication date: 20160504 |