CN109850947A - A kind of method that 12 hetropoly acid ammonium prepares molybdenum disulfide particle - Google Patents
A kind of method that 12 hetropoly acid ammonium prepares molybdenum disulfide particle Download PDFInfo
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- CN109850947A CN109850947A CN201910224140.XA CN201910224140A CN109850947A CN 109850947 A CN109850947 A CN 109850947A CN 201910224140 A CN201910224140 A CN 201910224140A CN 109850947 A CN109850947 A CN 109850947A
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- CN
- China
- Prior art keywords
- acid
- molybdenum disulfide
- molybdenum
- sulfide
- hetropoly
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- 239000002253 acid Substances 0.000 title claims abstract description 31
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 25
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 title claims abstract description 18
- 239000002245 particle Substances 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims abstract description 14
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 15
- 239000011733 molybdenum Substances 0.000 claims abstract description 15
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 239000003054 catalyst Substances 0.000 claims abstract description 8
- 239000003513 alkali Substances 0.000 claims abstract description 6
- 238000002425 crystallisation Methods 0.000 claims abstract description 6
- 230000008025 crystallization Effects 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 4
- 238000006479 redox reaction Methods 0.000 claims abstract description 3
- 238000002955 isolation Methods 0.000 claims abstract 2
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 7
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical group CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 6
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 3
- 239000011574 phosphorus Substances 0.000 claims description 3
- 229910052698 phosphorus Inorganic materials 0.000 claims description 3
- 229910009112 xH2O Inorganic materials 0.000 claims description 3
- 238000005461 lubrication Methods 0.000 claims description 2
- 238000004073 vulcanization Methods 0.000 claims 1
- 239000000314 lubricant Substances 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 3
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 238000001035 drying Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 150000003797 alkaloid derivatives Chemical class 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- TVWWSIKTCILRBF-UHFFFAOYSA-N molybdenum trisulfide Chemical compound S=[Mo](=S)=S TVWWSIKTCILRBF-UHFFFAOYSA-N 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Landscapes
- Lubricants (AREA)
- Catalysts (AREA)
Abstract
A kind of method that 12 hetropoly acid ammonium prepares molybdenum disulfide particle, is related to lubricant and catalyst preparation technical field.First molybdenum source is dissolved with lye, then it is sufficiently mixed under the conditions of agitating and heating with sulfide solution, it is subsequently added into acid and neutralizes excessive alkali, and it adjusts and arrives pH value to acidity, then redox reaction occurs using the oxidisability of molybdenum source and the sulfide with reproducibility, it is dry after being separated by filtration after reaction, it is finally placed in isolation air heating crystallization, obtains the molybdenum disulfide particle that can be used for catalyst, solid lubricant.It is raw material that the present invention, which selects the 12 hetropoly acid ammoniums for being insoluble in water and strong acid, utilize processing mode sour after first alkali, its oxidisability direct oxidation sulfide is recycled, while itself being reduced into Mo (VI), is finally precipitated out in the form of molybdenum disulfide.There are higher potential using values in the fields such as lubricant and catalyst for the molybdenum disulfide particle of preparation.
Description
Technical field
The present invention relates to lubricants and catalyst preparation technical field, are specifically related to a kind of 12 hetropoly acid ammonium systems
The method of standby molybdenum disulfide particle.
Background technique
12 hetropoly acid ammonium (H12Mo12N3O40) or its hydrate (H P12Mo12N3O40P·xH2O) dissolution in water
Very little is spent, can be dissolved in alkali.It is mainly used for phosphorus and exchanges reagent etc. with the analysis of tin, alkaloid reagent and cation.
Molybdenum disulfide has excellent lubrication and catalytic performance, its performance is related with the size that it forms particle, generally
Better performances when size is smaller, so that the preparation of molybdenum disulfide particle be made to be taken seriously.Preparation method mainly has following several at present
Kind, first is that reacting using soluble molybdate with sulfide, molybdenum trisulfide is generated, then heated desulfurization obtains curing again
Molybdenum nanoparticle；It is also to be reduced directly molybdate using hydrothermal synthesis method using sulfide, generate molybdenum disulfide.These
The disadvantages of all there is manufacturing cost height in preparation method, reaction step is many and diverse.
Summary of the invention
The technical problem to be solved by the present invention is to propose that a kind of 12 hetropoly acid ammoniums prepare the side of molybdenum disulfide particle
Method.
To achieve the goals above, the technical scheme adopted by the invention is as follows: a kind of 12 hetropoly acid ammoniums preparation two
The method for vulcanizing molybdenum particles, molybdenum source is first dissolved with lye, be then sufficiently mixed under the conditions of agitating and heating with sulfide solution,
It is subsequently added into the excessive alkali of acid neutralization, and is adjusted to pH value to acidity, the oxidisability of molybdenum source is then utilized and there is reproducibility
Redox reaction occurs for sulfide, dry after being separated by filtration after reaction, is finally placed at 300~500 DEG C and completely cuts off sky
Gas heating crystallization obtains the molybdenum disulfide particle that can be used for catalyst, solid lubricant.
The optimal technical scheme of the method for molybdenum disulfide particle is prepared as 12 hetropoly acid ammoniums of the invention, is prepared
In method:
The molybdenum source is 12 hetropoly acid ammonium H12Mo12N3O40P or its hydrate H12Mo12N3O40P·xH2O。
The sulfide is thioacetamide, mass ratio 1:1.5~2.5 of molybdenum source and sulfide.
The lye is the potassium hydroxide solution that concentration is 10~15%, and molybdenum source and lye mass ratio are 1:25~50.
The acid is the hydrochloric acid or phosphoric acid solution that concentration is 4~7mol/L, adjusts pH value of reaction system < 4 by acid.
Compared with prior art, beneficial effects of the present invention are shown:
It is raw material that the present invention, which has abandoned common soluble molybdenum hydrochlorate, also without selecting difficult industrialized hydrothermal synthesis method,
And the 12 hetropoly acid ammoniums for being insoluble in water and strong acid is selected to recycle it using processing mode sour after first alkali for raw material
Oxidisability direct oxidation sulfide, while itself being reduced into Mo (VI), be finally precipitated out in the form of molybdenum disulfide.It belongs to
It is easy to operate in liquid-phase precipitation method, it is suitble to amplification production.The molybdenum disulfide particle of preparation is deposited in the fields such as lubricant and catalyst
In higher potential using value.
Detailed description of the invention
Prepared by molybdenum disulfide particle to 12 hetropoly acid ammonium of one kind of the invention with attached drawing with reference to embodiments
Method, which is made, to be discussed further.
Fig. 1 is the XRD spectrum that embodiment 1 prepares product.
Fig. 2 is the scanning electron microscope (SEM) photograph that embodiment 1 prepares product.
Specific embodiment
Embodiment 1
The 12 hetropoly acid ammoniums for weighing 1.5g, be dissolved in 50g, 12% potassium hydroxide solution in, in heating stirring
It is lower to be sufficiently mixed the thioacetamide of 3g and above-mentioned solution, then with the salt acid for adjusting pH value of 5.5mol/L to 4, reaction terminates
Afterwards, obtained precipitated product is washed and obtains molybdenum disulfide with after drying through filtering, be then used as after 480 DEG C of heating crystallizations and urge
Agent.
Fig. 1,2 are to react to prepare molybdenum disulfide with thioacetamide using 12 hetropoly acid ammoniums in embodiment 1 respectively
The XRD spectrum of obtained product, scanning electron microscope (SEM) photograph.Molybdenum disulfide particle can be belonged to by having 4 in Fig. 1 in main diffraction peak
(002), (100), (103), (110) show that molybdenum disulfide is successfully prepared.Fig. 2 shows that molybdenum disulfide is graininess, particle
Average-size is less than 100 nanometers.
Embodiment 2
The 12 hetropoly acid ammoniums for weighing 1.5g, be dissolved in 75g, 10% potassium hydroxide solution in, in heating stirring
It is lower to be sufficiently mixed the thioacetamide of 3.75g and above-mentioned solution, then with the phosphorus acid for adjusting pH value of 4mol/L to 3, reaction terminates
Afterwards, obtained precipitated product is washed and obtains molybdenum disulfide with after drying through filtering, be then used as after 300 DEG C of heating crystallizations solid
Body lubricant.
Embodiment 3
The 12 hetropoly acid ammoniums for weighing 1.5g, be dissolved in 37.5g, 15% potassium hydroxide solution in, stirred in heating
Mix it is lower the thioacetamide of 2.25g and above-mentioned solution are sufficiently mixed, then with the salt acid for adjusting pH value of 7mol/L to 3.5, reaction
After, the washing of obtained precipitated product is obtained into molybdenum disulfide with after drying through filtering, is then used after 500 DEG C of heating crystallizations
Make catalyst.
The above content is just an example and description of the concept of the present invention, affiliated those skilled in the art
It makes various modifications or additions to the described embodiments or is substituted in a similar manner, without departing from invention
Design or beyond the scope defined by this claim, be within the scope of protection of the invention.
Claims (5)
1. a kind of method that 12 hetropoly acid ammoniums prepare molybdenum disulfide particle, which is characterized in that first with lye that molybdenum source is molten
Solution, is then sufficiently mixed under the conditions of agitating and heating with sulfide solution, is subsequently added into acid and neutralizes excessive alkali, and adjusts and arrive pH
Then using the oxidisability of molybdenum source and the sulfide with reproducibility redox reaction occurs for value, after reaction to acidity
It is dry after being separated by filtration, it is finally placed in isolation air heating crystallization at 300~500 DEG C, obtains can be used for catalyst, solid profit
The molybdenum disulfide particle of lubrication prescription.
2. preparation method as claimed in claim 2, which is characterized in that the molybdenum source is 12 hetropoly acid ammoniums
H12Mo12N3O40P or its hydrate H12Mo12N3O40P·xH2O。
3. preparation method as claimed in claim 2, which is characterized in that the sulfide is thioacetamide, molybdenum source and vulcanization
Mass ratio 1:1.5~2.5 of object.
4. preparation method as claimed in claim 2, which is characterized in that the lye is the potassium hydroxide that concentration is 10~15%
Solution, molybdenum source and lye mass ratio are 1:25~50.
5. preparation method as claimed in claim 2, which is characterized in that the acid is the hydrochloric acid or phosphorus that concentration is 4~7mol/L
Acid solution adjusts pH value of reaction system < 4 by acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910224140.XA CN109850947B (en) | 2019-03-22 | 2019-03-22 | Method for preparing molybdenum disulfide particles from ammonium dodecamolybdenum phosphapolyate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910224140.XA CN109850947B (en) | 2019-03-22 | 2019-03-22 | Method for preparing molybdenum disulfide particles from ammonium dodecamolybdenum phosphapolyate |
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| Publication Number | Publication Date |
|---|---|
| CN109850947A true CN109850947A (en) | 2019-06-07 |
| CN109850947B CN109850947B (en) | 2021-09-21 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910224140.XA Active CN109850947B (en) | 2019-03-22 | 2019-03-22 | Method for preparing molybdenum disulfide particles from ammonium dodecamolybdenum phosphapolyate |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101024517A (en) * | 2007-01-30 | 2007-08-29 | 合肥工业大学 | Method for preparing non-crystal molybdemum sulfide nano powder |
| 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 with layered shell structure |
| 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 | Method for preparing molybdenum disulfide nanoparticles with controllable 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 |
-
2019
- 2019-03-22 CN CN201910224140.XA patent/CN109850947B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 with layered shell 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 | Method for preparing molybdenum disulfide nanoparticles with controllable 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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| CN109850947B (en) | 2021-09-21 |
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