CN109850947B - Method for preparing molybdenum disulfide particles from ammonium dodecamolybdenum phosphapolyate - Google Patents
Method for preparing molybdenum disulfide particles from ammonium dodecamolybdenum phosphapolyate Download PDFInfo
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Abstract
A method for preparing molybdenum disulfide particles from ammonium dodecamolybdenum phosphapolyacid relates to the technical field of lubricant and catalyst preparation. Dissolving a molybdenum source by using alkali liquor, then fully mixing the molybdenum source with a sulfide solution under stirring and heating conditions, adding acid to neutralize excessive alkali, adjusting the pH value to acidity, then carrying out redox reaction on the molybdenum source and the sulfide with reducibility by using the oxidability of the molybdenum source, filtering and separating the molybdenum source after the reaction is finished, drying the molybdenum source, and finally placing the molybdenum source in isolated air for heating and crystallization to obtain molybdenum disulfide particles which can be used as a catalyst and a solid lubricant. The method selects the dodecamolybdenum ammonium phosphoheteropoly acid which is difficult to dissolve in water and strong acid as raw materials, utilizes the treatment mode of firstly alkali and then acid, and then utilizes the oxidizability of the dodecamolybdenum ammonium phosphoheteropoly acid to directly oxidize sulfide, and simultaneously, the dodecamolybdenum ammonium phosphoheteropoly acid is reduced into Mo (VI) and finally precipitated in the form of molybdenum disulfide. The prepared molybdenum disulfide particles have high potential application value in the fields of lubricants, catalysts and the like.
Description
Technical Field
The invention relates to the technical field of lubricant and catalyst preparation, in particular to a method for preparing molybdenum disulfide particles from ammonium dodecamolybdenum phosphapolyacid.
Background
Ammonium dodecamolybdenum phosphapolyate (H)12Mo12N3O40P) or hydrates thereof (H)12Mo12N3O40P·xH2O) has a very low solubility in water and is soluble in alkali. The method is mainly used for analyzing phosphorus and tin, alkaloid reagents, cation exchange reagents and the like.
Molybdenum disulfide has excellent lubricating and catalytic properties, the performance of the molybdenum disulfide is related to the size of particles formed by the molybdenum disulfide, and the performance is better when the molybdenum disulfide is smaller, so that the preparation of the molybdenum disulfide particles is emphasized. Firstly, soluble molybdate is utilized to react with sulfide to generate molybdenum trisulfide, and then the molybdenum trisulfide is heated and desulfurized to obtain molybdenum disulfide nanoparticles; and in addition, the molybdenum disulfide is generated by directly reducing molybdate by using sulfide by using a hydrothermal synthesis method. These preparation methods have the disadvantages of high production cost, complicated reaction steps, and the like.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for preparing molybdenum disulfide particles by ammonium dodecamolybdenum phospha polyacid.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: dissolving a molybdenum source by using alkali liquor, then fully mixing the molybdenum source with a sulfide solution under stirring and heating conditions, adding acid to neutralize excessive alkali, adjusting the pH value to acidity, then performing oxidation-reduction reaction on the molybdenum source and a sulfide with reducibility, filtering and separating after the reaction is finished, drying, and finally placing at 300-500 ℃ to isolate air for heating crystallization to obtain the molybdenum disulfide particles used for catalysts and solid lubricants.
As a preferred technical scheme of the method for preparing the molybdenum disulfide particles by the ammonium dodecamolybdenum phosphapolyacid, the preparation method comprises the following steps:
the molybdenum source is dodecamolybdenum phosphorus heteropoly acid ammonium H12Mo12N3O40P or hydrate H thereof12Mo12N3O40P·xH2O。
The sulfide is thioacetamide, and the mass ratio of the molybdenum source to the sulfide is 1: 1.5 to 2.5.
The alkali liquor is a potassium hydroxide solution with the concentration of 10-15%, and the mass ratio of the molybdenum source to the alkali liquor is 1: 25 to 50.
The acid is a hydrochloric acid or phosphoric acid solution with the concentration of 4-7 mol/L, and the pH value of the reaction system is adjusted to be less than 4 through the acid.
Compared with the prior art, the invention has the beneficial effects that:
the invention abandons the common soluble molybdate as the raw material, does not select a hydrothermal synthesis method which is difficult to industrialize, selects the dodecamolybdenum phosphoheteropoly acid ammonium which is difficult to dissolve in water and strong acid as the raw material, utilizes the treatment mode of firstly alkali and then acid, then utilizes the oxidizability thereof to directly oxidize sulfide, and simultaneously, the dodecamolybdenum phosphoheteropoly acid ammonium is reduced into Mo (VI) and finally precipitated in the form of molybdenum disulfide. It belongs to a liquid phase precipitation method, has simple operation and is suitable for large-scale production. The prepared molybdenum disulfide particles have high potential application value in the fields of lubricants, catalysts and the like.
Drawings
The method for preparing molybdenum disulfide particles by using ammonium dodecamolybdophosphates according to the present invention is further described in detail with reference to the following examples and accompanying drawings.
Figure 1 is the XRD pattern of the product prepared in example 1.
FIG. 2 is a scanning electron micrograph of the product prepared in example 1.
Detailed Description
Example 1
Weighing 1.5g of ammonium dodecamolybdenum phosphoheteropoly acid, dissolving in 50g of 12% potassium hydroxide solution, fully mixing 3g of thioacetamide with the solution under heating and stirring, adjusting the pH value to 4 by using 5.5mol/L hydrochloric acid, washing an obtained precipitation product after reaction is finished, filtering and drying to obtain molybdenum disulfide, and heating and crystallizing at 480 ℃ to be used as a catalyst.
Fig. 1 and 2 are respectively an XRD spectrum and a scanning electron microscope image of a product obtained by preparing molybdenum disulfide by reacting ammonium dodecamolybdophosphates with thioacetamide in example 1. In fig. 1, 4 of the main diffraction peaks can be assigned to (002), (100), (103), (110) of the molybdenum disulfide particles, indicating that molybdenum disulfide has been successfully produced. Figure 2 shows that the molybdenum disulphide is in particulate form with particles having an average size of less than 100 nm.
Example 2
Weighing 1.5g of ammonium dodecamolybdophosphoric polyacid, dissolving in 75g of 10% potassium hydroxide solution, fully mixing 3.75g of thioacetamide with the solution under heating and stirring, adjusting the pH value to 3 by using 4mol/L phosphoric acid, washing an obtained precipitate after the reaction is finished, filtering and drying to obtain molybdenum disulfide, and then heating and crystallizing at 300 ℃ to be used as a solid lubricant.
Example 3
Weighing 1.5g of ammonium dodecamolybdophosphoric polyacid, dissolving in 37.5g of 15% potassium hydroxide solution, fully mixing 2.25g of thioacetamide with the solution under heating and stirring, adjusting the pH value to 3.5 by using 7mol/L hydrochloric acid, washing an obtained precipitate after the reaction is finished, filtering and drying to obtain molybdenum disulfide, and then heating and crystallizing at 500 ℃ to be used as a catalyst.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.
Claims (3)
1. A method for preparing molybdenum disulfide particles from ammonium dodecamolybdate-phosphapolyacrylate is characterized by comprising the steps of dissolving a molybdenum source by using an alkali liquor, then fully mixing the molybdenum source with a sulfide solution under stirring and heating conditions, adding an acid to neutralize excessive alkali, adjusting the pH value to acidity, then carrying out redox reaction on the molybdenum source and a sulfide with reducibility by using the oxidability of the molybdenum source, filtering and separating the molybdenum source after the reaction is finished, drying the molybdenum source, and finally placing the molybdenum source at 300-500 ℃ to isolate air for heating crystallization to obtain the molybdenum disulfide particles used for catalysts and solid lubricants;
the molybdenum source is dodecamolybdenum phosphorus heteropoly acid ammonium H12Mo12N3O40P or hydrate H thereof12Mo12N3O40P·xH2O, the sulfide is thioacetamide, and the mass ratio of the molybdenum source to the sulfide is 1: 1.5 to 2.5.
2. The preparation method of claim 1, wherein the alkali liquor is a potassium hydroxide solution with a concentration of 10-15%, and the mass ratio of the molybdenum source to the alkali liquor is 1: 25 to 50.
3. The preparation method according to claim 1, wherein the acid is a hydrochloric acid or phosphoric acid solution with a concentration of 4-7 mol/L, and the pH value of the reaction system is adjusted to be less than 4 by the acid.
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| CN101024517A (en) * | 2007-01-30 | 2007-08-29 | 合肥工业大学 | Method for preparing non-crystal molybdemum sulfide nano powder |
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| CN105731542A (en) * | 2014-12-10 | 2016-07-06 | 中国科学院大连化学物理研究所 | A method of preparing molybdenum disulfide microspheres in a reversed-phase microemulsion system |
| CN106629852A (en) * | 2016-12-10 | 2017-05-10 | 浙江大学 | Preparation method of multilayer molybdenum disulfide material |
| CN106986386A (en) * | 2017-05-03 | 2017-07-28 | 合肥学院 | A kind of controllable method for preparing molybdenum disulfide nano particulate of product form |
| CN108217728A (en) * | 2016-12-09 | 2018-06-29 | 中国科学院大连化学物理研究所 | A kind of MoS2Nano-particle morphology controllable preparation method |
| CN109437307A (en) * | 2018-12-19 | 2019-03-08 | 王子韩 | A kind of method of efficient preparation high quality molybdenum disulfide nano line |
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- 2019-03-22 CN CN201910224140.XA patent/CN109850947B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101024517A (en) * | 2007-01-30 | 2007-08-29 | 合肥工业大学 | Method for preparing non-crystal molybdemum sulfide nano powder |
| CN105731542A (en) * | 2014-12-10 | 2016-07-06 | 中国科学院大连化学物理研究所 | A method of preparing molybdenum disulfide microspheres in a reversed-phase microemulsion system |
| CN105366726A (en) * | 2015-12-16 | 2016-03-02 | 中国科学院理化技术研究所 | Preparation method of hollow spherical molybdenum disulfide of laminated shell layer structure |
| CN108217728A (en) * | 2016-12-09 | 2018-06-29 | 中国科学院大连化学物理研究所 | A kind of MoS2Nano-particle morphology controllable preparation method |
| CN106629852A (en) * | 2016-12-10 | 2017-05-10 | 浙江大学 | Preparation method of multilayer molybdenum disulfide material |
| CN106986386A (en) * | 2017-05-03 | 2017-07-28 | 合肥学院 | A kind of controllable method for preparing molybdenum disulfide nano particulate of product form |
| CN109437307A (en) * | 2018-12-19 | 2019-03-08 | 王子韩 | A kind of method of efficient preparation high quality molybdenum disulfide nano line |
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