CN111233040A - Method for preparing nano molybdenum disulfide by solvothermal method, catalyst and application - Google Patents
Method for preparing nano molybdenum disulfide by solvothermal method, catalyst and application Download PDFInfo
- Publication number
- CN111233040A CN111233040A CN201811441057.XA CN201811441057A CN111233040A CN 111233040 A CN111233040 A CN 111233040A CN 201811441057 A CN201811441057 A CN 201811441057A CN 111233040 A CN111233040 A CN 111233040A
- Authority
- CN
- China
- Prior art keywords
- mos
- catalyst
- molybdenum
- nano
- hours
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/06—Sulfides
-
- 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
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention discloses a solvothermal preparation method of high-activity molybdenum disulfide (MoS)2) The method for preparing the catalyst comprises the steps of taking molybdenum oxide or molybdate as a molybdenum source, taking L-cysteine or glutathione as a sulfur source, and preparing the nano MoS by solvothermal method2. The MoS provided by the invention2The preparation method of the catalyst is simple, mild in condition and suitable for large-scale preparation. The MoS2The catalyst is used in the catalytic hydrogenation process of polycyclic aromatic hydrocarbon, shows excellent catalytic performance, is not easy to be poisoned, and is expected to be used in the actual oil hydrogenation process.
Description
Technical Field
The invention belongs to the field of inorganic nano material synthesis, and particularly relates to a method for solvothermal synthesis of nano molybdenum disulfide and application of nano molybdenum disulfide in polycyclic aromatic hydrocarbon hydrogenation.
Background
MoS2Is the main component of molybdenite, and a sandwich type slab layer exists in the crystal structure: two layers of S atoms sandwich one layer of Mo atoms to form a sandwich structure. The atoms in the layers are bonded by strong covalent bonds, the van der waals force between the layers is weak, the layers are easy to peel, and the film has good anisotropy and low friction factor. MoS2Are widely used hydrogenation catalysts whose active sites are the Rim and Edge sites at the edges of the layer (see r. chianelli. journal of catalysis,1994,149, 414-427.). The conventional catalyst is a massive MoS2The granule is characterized by large particle size, small specific surface and low utilization rate of active components. Preparation of nanoscale MoS2The catalyst can greatly increase the number of edge sites and improve the hydrogenation activity.
At present, MoS2Synthetic methods can be broadly divided into three major categories: high-temperature gas-solid phase synthesis method, physical synthesis method and wet chemical synthesis method. Feldman et al, in the Science journal of 1995 (267 Vol., page 222), published a method of heating MoO in a tube furnace3Heating to 850 deg.C, introducing H2S(H2+N2) Reducing gas, MoO in a high temperature reducing atmosphere3And H2S gas reacts to prepare MoS2Fullerene nanoparticles and nanotubes. Patent US4243553A l discloses a MoS for preparing high specific surface2The method is characterized in that the thiomolybdate is calcined at a high temperature of 300-800 ℃ in an inert atmosphere. The gas-solid method has harsh preparation conditions, has higher requirements on equipment environment and needs to use toxic gas H2S, and the like, and the obtained product is not easy to disperse. The physical method is to carry out MoS treatment by means of mechanical grinding, ultrasonic stripping and the like2Is crushed, cut orStripping to refine or obtain MoS2Purpose of nanosheet. Patent CN 107500358A discloses ultrasonic exfoliation of powdered MoS with an organic solvent with addition of an inorganic salt2Obtaining single-layer or few-layer MoS2A method of nanoplatelets. The method has the advantages of complex operation and small preparation amount, and is not suitable for large-scale production.
The wet chemical synthesis method has the advantages of mild conditions and simple operation, and is an advantageous synthesis method. Patent CN106145190A discloses that precursor formed by molybdate poly-acid salt and imidazole ionic liquid thioamide grows in an oriented way and is decomposed in a sulfuration way under the in-situ condition so as to realize MoS self-assembled by ultrathin nanosheets2A method of nanotubes. The patent CN105776335B discloses a method for preparing high-purity phase spherical MoS by dissolving ammonium heptamolybdate, thioacetamide and surfactant in a solvent and carrying out hydrothermal synthesis2The method of (1). Patent CN105366725B discloses a hydro-thermal synthesis MoS using sulfur-containing biological reagent as sulfur source2In the method for preparing the nanoflower, the sulfur-containing biological reagent is a mild and safe sulfur source, and no additional reducing agent is needed in the synthesis process. In the hydrothermal or solvothermal process, conditions such as a sulfur source, a molybdenum source, a solvent, pH and the like have great influence on the structure, the size and the appearance of a product. However, the nano-scale product of the hydrothermal synthesis is easy to agglomerate, and the size and the shape are difficult to control. The selection of a suitable solvent is therefore of critical importance.
Disclosure of Invention
The invention aims to solve the problems and provides a method for preparing high-dispersion MoS by solvothermal method2The preparation method of the catalyst is applied to the catalytic hydrogenation process of the polycyclic aromatic hydrocarbon.
The MoS provided by the invention2The preparation method of the catalyst is a solvent thermosynthesis method: adding a sulfur source and a molybdenum source into a solvent, stirring at the speed of 300-500 rpm for 5-30 min, transferring into a high-pressure reaction kettle, sealing, and placing in an oven for hydrothermal reaction at 120-200 ℃ for 12-48 hours. Centrifuging at the speed of 3000-5000 rpm to obtain black precipitates, washing the precipitates with deionized water and absolute ethyl alcohol, and drying in vacuum to obtain black powdery samples.
The molybdenum source is one or a mixture of two or a mixture of three of molybdenum trioxide, ammonium heptamolybdate and molybdic acid, and molybdenum trioxide is preferred.
The sulfur source is L-cysteine or glutathione or a mixture of the two, preferably L-cysteine. The concentration of the sulfur source in the solution is 0.02-0.5 mol/L, preferably 0.05-0.15 mol/L, and the molar ratio of S/Mo in the raw material is 10: 1-2: 1.
The solvent is ethanol or a mixed solvent of ethanol and water, and the volume ratio of the water to the ethanol is preferably 0-3, and most preferably 0.5-1.5.
The stirring speed is 300-500 rpm, preferably 300-400 rpm, and the stirring time is 5-30 min, preferably 10-20 min.
The temperature of the hydrothermal reaction in the step is 120-240 ℃, preferably 160-200 ℃, and the reaction time is 12-48 hours, preferably 16-24 hours.
The centrifugal separation speed is 3000-5000 rpm, and preferably 4000-4500 rpm.
The vacuum drying conditions are as follows: temperature 40-70 ℃, preferably 60-70 ℃, time: 6 to 14 hours, preferably 8 to 12 hours.
The invention has the following advantages:
(1) MoS prepared by the invention2The process has simple operation, mild reaction condition and MoS2The yield is high. The sulfur source is a vulcanizing agent and a reducing agent, and no additional reducing agent is needed.
(2) The solvent adopted by the invention effectively regulates and controls the crystallization nucleation quantity and speed and the diffusion speed in the synthesis process, and the high-activity-site-exposed nano MoS is prepared2And (4) preparing a hydrogenation catalyst.
(3) MoS prepared by the invention2Consists of a large number of nano sheets, the nano sheets are highly dispersed, stacking is not formed, and MoS is increased2And (4) exposing active sites.
(4) The nano MoS synthesized by the invention2The hydrogenation catalyst has very high catalytic hydrogenation activity when being used in hydrogenation reaction of polycyclic aromatic hydrocarbon compounds, is not easy to be poisoned, and is expected to be used in preparing clean fuel by hydrogenation of real oil products.
Drawings
FIG. 1 shows the nano-MoS obtained in example 12XRD spectrum of catalyst, commercial MoS2As a control;
FIG. 2a shows the nano-MoS obtained in example 12Low power transmission electron microscope images of the catalyst;
FIG. 2b shows the nano-MoS obtained in example 12High power transmission electron microscope images of the catalyst;
the present invention is further illustrated in detail below with reference to table 1 and examples.
Example 1
Weighing 16mmol L-cysteine, dissolving in 50ml mixed solution of water and ethanol (V)Water (W)/(VEthanol+VWater (W)) 0.3), a 0.32mol/L solution was formed, and 2mmol of molybdenum trioxide was further added. And (3) after fully stirring, transferring the suspension into a 100ml high-pressure reaction kettle, carrying out hydrothermal reaction at 200 ℃ for 16 hours, naturally cooling, carrying out suction filtration, washing the precipitate with deionized water and absolute ethyl alcohol, and then carrying out vacuum drying at 70 ℃ for 12 hours to obtain black powder. XRD characterization showed the resulting black powder to be MoS2The diffraction peak width becomes larger, indicating that the MoS was obtained2The size is small (see fig. 1). The calculated S-Mo-S interlayer spacing was 0.96nm, compared to the standard MoS2The S-Mo-S interlayer spacing of 0.62nm is obviously increased. Transmission electron microscope images show the MoS prepared2The nano-film consists of a large number of nano-sheets (see figure 2a), the number of S-Mo-S molecular layers is 2-3, and the interlayer spacing is enlarged to 0.96nm (see figure 2 b). The length of the nano-sheet is only 10-20 nm, and a large number of edge positions exist, and the edge positions are MoS2The hydrogenation active site of (3).
Example 2
8mmol of L-cysteine was weighed into 50ml of ethanol to form a 0.16mol/L solution, and 2mmol of molybdic acid was added. And (3) transferring the solution into a high-pressure reaction kettle after fully stirring, carrying out hydrothermal reaction at 200 ℃ for 22 hours, naturally cooling, carrying out suction filtration, washing the precipitate with deionized water and absolute ethyl alcohol, and then carrying out vacuum drying at 70 ℃ for 12 hours to obtain black powder. XRD characterization showed the resulting black powder to be an interlayer spacing expanded MoS2. Transmission electron microscope images show the MoS prepared2The nano-film is composed of a large number of nano-sheets, the number of S-Mo-S molecular layers is 2-3, and the interlayer spacing is enlarged to 0.96 nm. The length of the nano-sheet is only 5-15 nm, and a large number of edge positions exist, and the edge positions are MoS2The hydrogenation active site of (3).
Example 3
8mmol of L-cysteine was weighed out and dissolved in 50ml of deionized water to form a 0.16mol/L solution, and 2mmol of ammonium heptamolybdate was added. And (3) transferring the solution into a high-pressure reaction kettle after fully stirring, carrying out hydrothermal reaction at 200 ℃ for 22 hours, naturally cooling, carrying out suction filtration, washing the precipitate with deionized water and absolute ethyl alcohol, and then carrying out vacuum drying at 70 ℃ for 12 hours to obtain black powder. XRD characterization showed the resulting black powder to be an interlayer spacing expanded MoS2. Transmission electron microscope images show the MoS prepared2The nano-film is composed of a large number of nano-sheets, the number of S-Mo-S molecular layers is 2-3, and the interlayer spacing is enlarged to 0.96 nm. The length of the nano-sheet is only 5-15 nm, and a large number of edge positions exist, and the edge positions are MoS2The hydrogenation active site of (3).
Example 4
16mmol of L-cysteine was weighed out and dissolved in 50ml of deionized water to form a 0.32mol/L solution, and 2mmol of molybdenum trioxide was added. And (3) after fully stirring, transferring the suspension into a 100ml high-pressure reaction kettle, carrying out hydrothermal reaction at 180 ℃ for 24 hours, naturally cooling, carrying out suction filtration, washing the precipitate with deionized water and absolute ethyl alcohol, and then carrying out vacuum drying at 70 ℃ for 8 hours to obtain black powder. XRD characterization showed the resulting black powder to be an interlayer spacing expanded MoS2。
Example 5
16mmol of L-cysteine was weighed out and dissolved in 50ml of deionized water to form a 0.32mol/L solution, and 2mmol of molybdenum trioxide was added. And (3) after fully stirring, transferring the suspension into a 100ml high-pressure reaction kettle, carrying out hydrothermal reaction at 180 ℃ for 24 hours, naturally cooling, carrying out suction filtration, washing the precipitate with deionized water and absolute ethyl alcohol, and then carrying out vacuum drying at 60 ℃ for 12 hours to obtain black powder. XRD characterization showed the resulting black powder to be an interlayer spacing expanded MoS2。
Example 6
Weighing 16mmol glutathione and dissolving in 50mTo deionized water, a solution of 0.32mol/L was formed, and 2mmol of molybdenum trioxide was added. And (3) after fully stirring, transferring the suspension into a 100ml high-pressure reaction kettle, carrying out hydrothermal reaction at 180 ℃ for 24 hours, naturally cooling, carrying out suction filtration, washing the precipitate with deionized water and absolute ethyl alcohol, and then carrying out vacuum drying at 70 ℃ for 12 hours to obtain black powder. XRD characterization showed the resulting black powder to be an interlayer spacing expanded MoS2。
Example 7
16mmol of glutathione was weighed out and dissolved in 50ml of deionized water to form a 0.32mol/L solution, and 2mmol of molybdenum trioxide was added. And (3) after fully stirring, transferring the suspension into a 100ml high-pressure reaction kettle, carrying out hydrothermal reaction at 180 ℃ for 24 hours, naturally cooling, carrying out suction filtration, washing the precipitate with deionized water and absolute ethyl alcohol, and then carrying out vacuum drying at 70 ℃ for 12 hours to obtain black powder. XRD characterization showed the resulting black powder to be an interlayer spacing expanded MoS2。
Example 8
16mmol of glutathione was weighed out and dissolved in 50ml of deionized water to form a 0.32mol/L solution, and 2mmol of ammonium heptamolybdate was added. And (3) after fully stirring, transferring the suspension into a 100ml high-pressure reaction kettle, carrying out hydrothermal reaction at 180 ℃ for 24 hours, naturally cooling, carrying out suction filtration, washing the precipitate with deionized water and absolute ethyl alcohol, and then carrying out vacuum drying at 70 ℃ for 12 hours to obtain black powder. XRD characterization showed the resulting black powder to be an interlayer spacing expanded MoS2。
Example 9
The products prepared in examples 1-8 were used as catalysts for the performance evaluation of anthracene hydrogenation catalysts and for comparison with commercial molybdenum disulfide in the following steps: in a l00mL autoclave reactor of a suspended bed reaction system, 0.075g of MoS prepared in example 1 was charged2Catalyst (2.5% by weight, based on anthracene) was added with 3g of anthracene and 30g of n-tridecane. After the autoclave is installed, the air is replaced by hydrogen for 3 times (the tail gas valve is closed, then the gas inlet valve is opened, the pressure of the hydrogen at l00ml/min is increased to 2MPa, then the gas inlet valve is closed, then the tail gas valve is opened for emptying), the pressure is increased to 8MPa, stirring is started, and the stirring speed is 300 r/min. The timing is started when the temperature rises to 350 ℃ at the speed of 10 ℃/minAnd naturally cooling after keeping for 4 hours.
The result of the anthracene catalytic hydrogenation reaction comprises product selectivity, anthracene conversion rate and anthracene hydrogenation rate, and the hydrogenation products are respectively dihydroanthracene (H)2A) Tetrahydroanthracene (H)4A) Octahydro anthracene (H)8A) Tetradecahydroanthracene (H)14A)。
MoS of the invention2Catalysts were used in anthracene suspension bed hydrogenation reactions, MoS obtained in examples 1-82The hydrogenation rate and the selectivity of the octahydro anthracene which is a product of deep hydrogenation obtained by the catalyst are both higher than those of the commercial MoS2. The highest selectivity of the octahydroanthracene which is a deep hydrogenation product can reach 82.9 percent, and the octahydroanthracene is a commercial MoS27.0 times of catalyst: the hydrogenation rate can reach 55 percent at most, and the product is commercial MoS22.3 times higher (see table 1).
TABLE 1 MoS2Evaluation results of Anthracene-catalyzed hydrogenation of catalyst
Claims (10)
1. A method for preparing nano molybdenum disulfide by solvothermal method is characterized by comprising the following steps: the preparation steps are as follows: sequentially adding a sulfur source and a molybdenum source into a solvent, transferring the prepared solution or suspension into a high-pressure reaction kettle, sealing, carrying out solvothermal reaction, naturally cooling, separating a solid product, and drying in vacuum to obtain the nano MoS2A catalyst.
2. The method of claim 1, wherein: the molybdenum source is one of molybdenum trioxide, ammonium heptamolybdate and molybdic acid or a mixture of any two of the molybdenum trioxide, the ammonium heptamolybdate and the molybdic acid or a mixture of three of the molybdenum trioxide, the ammonium heptamolybdate and the molybdic acid;
the sulfur source is L-cysteine or glutathione or a mixture of the L-cysteine and the glutathione.
3. The method of claim 1, further comprising: the solvent is ethanol or a mixture of ethanol and water, and the volume concentration of the ethanol is 10-100%.
4. The method of claim 1, wherein: the concentration of the sulfur source in the solution is 0.02-0.5 mol/L.
5. The method according to claim 1 or 4, characterized in that: the molar ratio of S/Mo in the raw materials is 10: 1-2: 1.
6. The method of claim 1, wherein: the temperature of the hydrothermal reaction is 120-200 ℃, and the time is 12-48 hours.
7. The method of claim 1, wherein: the pH value of the suspension or the solution is 1-7, namely the reaction system is acidic or neutral.
8. The method of claim 1, wherein: the vacuum drying conditions in the step: temperature 40-70 ℃, time: 6 to 12 hours.
9. A catalyst obtained by the production method according to any one of claims 1 to 8.
10. The MoS of claim 92The application of the nano catalyst is characterized in that: the method is used for polycyclic aromatic hydrocarbon catalytic hydrogenation reaction.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811441057.XA CN111233040A (en) | 2018-11-29 | 2018-11-29 | Method for preparing nano molybdenum disulfide by solvothermal method, catalyst and application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811441057.XA CN111233040A (en) | 2018-11-29 | 2018-11-29 | Method for preparing nano molybdenum disulfide by solvothermal method, catalyst and application |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111233040A true CN111233040A (en) | 2020-06-05 |
Family
ID=70861622
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811441057.XA Pending CN111233040A (en) | 2018-11-29 | 2018-11-29 | Method for preparing nano molybdenum disulfide by solvothermal method, catalyst and application |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111233040A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112934244A (en) * | 2019-12-11 | 2021-06-11 | 中国科学院大连化学物理研究所 | Non-supported suspension bed hydrodesulfurization catalyst, preparation and application |
| CN114149592A (en) * | 2021-10-20 | 2022-03-08 | 江苏大学 | Composite ratiometric fluorescent probe and preparation method and application thereof |
| CN114392756A (en) * | 2022-01-26 | 2022-04-26 | 华中师范大学 | Preparation method of piezoelectric catalytic material, product and application thereof |
| CN114588921A (en) * | 2020-12-04 | 2022-06-07 | 中国科学院大连化学物理研究所 | Polycyclic aromatic hydrocarbon hydrogenation catalyst and polycyclic aromatic hydrocarbon hydrogenation reaction method |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2830394A1 (en) * | 1978-07-11 | 1980-01-31 | Elektrometallurgie Gmbh | Molybdenum oxide prodn. from molybdenum sulphide concentrate - by oxidn. in aq. slurry, with recirculation for higher yield and recovery of metallic impurities |
| CN101851006A (en) * | 2010-06-08 | 2010-10-06 | 南开大学 | Method for preparing MoS2 microspheres by solvent hot method |
| CN102698774A (en) * | 2012-06-08 | 2012-10-03 | 浙江大学 | Hydrothermal preparation method for single-layer MoS2 and graphene composite nano material |
| CN105366725A (en) * | 2014-08-29 | 2016-03-02 | 中国科学院大连化学物理研究所 | Method for hydro-thermally synthesizing MoS<2> nanoflower with sulfur-containing biological reagent as sulfur source |
| CN108715462A (en) * | 2018-08-31 | 2018-10-30 | 清华大学 | The method of the molybdenum disulfide particles of water/solvent-thermal process different morphologies |
-
2018
- 2018-11-29 CN CN201811441057.XA patent/CN111233040A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2830394A1 (en) * | 1978-07-11 | 1980-01-31 | Elektrometallurgie Gmbh | Molybdenum oxide prodn. from molybdenum sulphide concentrate - by oxidn. in aq. slurry, with recirculation for higher yield and recovery of metallic impurities |
| CN101851006A (en) * | 2010-06-08 | 2010-10-06 | 南开大学 | Method for preparing MoS2 microspheres by solvent hot method |
| CN102698774A (en) * | 2012-06-08 | 2012-10-03 | 浙江大学 | Hydrothermal preparation method for single-layer MoS2 and graphene composite nano material |
| CN105366725A (en) * | 2014-08-29 | 2016-03-02 | 中国科学院大连化学物理研究所 | Method for hydro-thermally synthesizing MoS<2> nanoflower with sulfur-containing biological reagent as sulfur source |
| CN108715462A (en) * | 2018-08-31 | 2018-10-30 | 清华大学 | The method of the molybdenum disulfide particles of water/solvent-thermal process different morphologies |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112934244A (en) * | 2019-12-11 | 2021-06-11 | 中国科学院大连化学物理研究所 | Non-supported suspension bed hydrodesulfurization catalyst, preparation and application |
| CN114588921A (en) * | 2020-12-04 | 2022-06-07 | 中国科学院大连化学物理研究所 | Polycyclic aromatic hydrocarbon hydrogenation catalyst and polycyclic aromatic hydrocarbon hydrogenation reaction method |
| CN114588921B (en) * | 2020-12-04 | 2023-06-20 | 中国科学院大连化学物理研究所 | Polycyclic aromatic hydrocarbon hydrogenation catalyst and polycyclic aromatic hydrocarbon hydrogenation reaction method |
| CN114149592A (en) * | 2021-10-20 | 2022-03-08 | 江苏大学 | Composite ratiometric fluorescent probe and preparation method and application thereof |
| CN114149592B (en) * | 2021-10-20 | 2023-01-17 | 江苏大学 | Composite ratiometric fluorescent probe and preparation method and application thereof |
| CN114392756A (en) * | 2022-01-26 | 2022-04-26 | 华中师范大学 | Preparation method of piezoelectric catalytic material, product and application thereof |
| CN114392756B (en) * | 2022-01-26 | 2024-01-19 | 华中师范大学 | Preparation method of piezoelectric catalytic material, product and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111233040A (en) | Method for preparing nano molybdenum disulfide by solvothermal method, catalyst and application | |
| Song et al. | Ultrathin MXene “bridge” to accelerate charge transfer in ultrathin metal-free 0D/2D black phosphorus/g-C3N4 heterojunction toward photocatalytic hydrogen production | |
| CN107376971B (en) | Synthetic method of graphite-like carbon nitride/molybdenum disulfide nano composite material | |
| CN108067257B (en) | Preparation method of high-activity-site-exposed nano molybdenum disulfide hydrogenation catalyst | |
| Li et al. | Synthesis of hexagonal and triangular Fe 3 O 4 nanosheets via seed-mediated solvothermal growth | |
| CN111229258A (en) | Preparation method of high-activity molybdenum sulfide hydrogenation catalyst | |
| CN108565434B (en) | Preparation method of tungsten disulfide/nitrogen and sulfur co-doped graphene compound | |
| CN109796044B (en) | Molybdenum disulfide, cobalt-modified molybdenum disulfide, Pd-loaded nanosheet, and synthesis method and application thereof | |
| CN105417581A (en) | Method for complexing hydrothermal synthesis of uniform flower-like MoS2 nanospheres | |
| WO2021147213A1 (en) | Core-shell iron-based catalyst used for direct production of aromatic hydrocarbons from syngas, and preparation method and application therefor | |
| CN108483502A (en) | A kind of preparation method and application of rhenium disulfide nanometer sheet | |
| CN109110816B (en) | Synthetic method of oil-soluble molybdenum disulfide | |
| CN108579750B (en) | Copper-doped Ni/SiO2Nano composite catalyst and preparation method thereof | |
| CN107433203A (en) | A kind of Z Scheme compound systems and preparation method and application | |
| CN108217728A (en) | A kind of MoS2Nano-particle morphology controllable preparation method | |
| Su et al. | Defect-driven electroless deposition and activation of platinum sites on ZnIn2S4 nanosheets for accelerated kinetics of photocatalytic hydrogen production | |
| CN106602083B (en) | A kind of method of hydro-thermal method synthesis Cu-N-C catalyst | |
| Panigrahi et al. | A novel route for the synthesis of nanotubes and fullerene-like nanostructures of molybdenum disulfide | |
| CN111233038A (en) | Spherical molybdenum disulfide, preparation method and application thereof | |
| CN112939081B (en) | Preparation method of cobalt-doped molybdenum disulfide with yolk-eggshell structure | |
| CN112844413A (en) | Preparation method and application of photocatalyst with sphalerite/wurtzite junction | |
| CN111233039B (en) | Rod-shaped molybdenum disulfide material and preparation and application thereof | |
| CN108085557B (en) | Carbon nanotubes enhances tungsten-cobalt carbide-vanadium carbide hard alloy manufacturing method and equipment | |
| WO2023015632A1 (en) | Carbon dioxide hydrogenation-based methanol preparation catalyst, and preparation method therefor and use thereof | |
| Zhang et al. | Fabrication of porous MoS2 with controllable morphology and specific surface area for hydrodeoxygenation |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200605 |
|
| RJ01 | Rejection of invention patent application after publication |