CN105060347A - Method for synthesizing ultrathin molybdenum disulfide nanocrystals - Google Patents
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Abstract
The invention discloses a method for synthesizing ultrathin molybdenum disulfide nanocrystals and belongs to the technical field of inorganic material preparation processes. According to the method, a molybdenum-containing inorganic salt and a sulfur-containing compound or sulfur powder are used as raw materials and have a reaction at the temperature of 160-300 DEG C for 30-120 min in a long-chain amine solvent and a long-chain fatty acid surfactant, experiment parameters such as the reactant molar ratio, the reactant concentration, the reaction temperature, the reaction time and the like are controlled, molybdenum disulfide nanocrystals which are well crystallized and have a few atomic layers (1-5 layers) are formed and can be well dispersed in a nonpolar solvent or base oil, and stable lubricating oil is formed. According to the method, raw materials are cheap and easy to obtain, the reaction time is short, the yield is high, instruments and equipment are simple, operation is convenient, safe and reliable, process repeatability is good, product quality is stable, and the method is suitable for industrial enlarged production.
Description
Technical field
The present invention relates to a kind of method of synthesizing ultra-thin molybdenum disulfide nano crystalline substance, belong to inorganic material preparation process technical field.
Background technology
Molybdenumdisulphide is used for lubricating oil and lubricating grease, is the antifriction of excellent performance, wear-resistant and extreme pressure material.Molybdenumdisulphide solid lubricant can (as 0.5% ~ 85%) be dispersed in lubricating grease, lubricating oil, water and organic solvent in certain proportion, also can be used alone, can also be modulated into various resin the surface treatment agent that coating is used as each metalloid, alloy component, stupalith.Since over half a century, molybdenumdisulphide obtains widespread use at the power lubrication such as bearing, gear, industrial manufacture view.For solving the low present situation of energy utilization rate, based on the lubricity of molybdenumdisulphide excellence, domestic and international scientific research personnel is carrying out synthesis and the applied research of novel molybdenumdisulphide always.The molybdenumdisulphide with a few atomic is in recent years because it is in energy utilization, and as electrochemistry produces hydrogen, photochemical catalyzing, the fields such as lithium ion battery receive the extensive concern of investigator.
Production has ultra-thin molybdenumdisulphide current mainly stripping method and the chemical Vapor deposition process of a few atomic (1-5 layer).Wherein stripping method is mainly divided into mechanically peel and chemical stripping.These method costs are higher, and operation sequence is complicated, and length consuming time, energy consumption is high, not easily carries out amplification industrial production.In this year, some research institutions have attempted utilizing wet chemical method to remove to synthesize the molybdenum disulfide nano crystalline substance (ChemistryofMaterials, 23 volumes, 3879-3885 page, 2011) with a few atomic.But the method needs extreme temperatures, and the molybdenumdisulphide crystallization of synthesis is poor, yields poorly, is unfavorable for promoting the use of.So in order to the ultra-thin molybdenumdisulphide realizing having a few atomic is in the industrial application as fields such as lubricating oil additives, study a kind of simple process, constant product quality, consuming time few, economy, the preparation method being easy to produce in batches is a challenge of chemical science and technology field face.
Summary of the invention
The object of the present invention is to provide a kind of synthetic method with the ultra-thin molybdenum disulfide nano crystalline substance of a few atomic, the method adopts raw material cheap and easy to get, utilize simple approach, can synthesize in a large number, to fill up the blank of the brilliant simple and easy preparation aspect of the ultra-thin molybdenum disulfide nano with a few atomic.Because the method is easy to amplify, regulation and control are convenient, excellent product performance, and Modulatory character is strong, has wide market outlook by fields such as lubricating oil additives.
Technical scheme of the present invention is as follows:
Synthesize a method for a few atomic molybdenum disulfide nano crystalline substance, it is characterized in that the method is carried out as follows:
1) in long-chain amine solvent, first add long-chain fat acid additive, then add containing molybdenum inorganic salt and sulfocompound, the mol ratio of two kinds of compounds is 0.1 ~ 10:1, and the total mass concentration of two kinds of compounds is 0.01 ~ 2.0 gram/ml solvent;
2) range of reaction temperature is 160 ~ 300 DEG C, and reaction time range is 30 ~ 120 minutes;
3) by products therefrom washing with alcohol, be scattered in hexanaphthene and preserve, or after drying, directly obtain molybdenum disulfide nano crystalline flour end.
In technique scheme, described long-chain amine solvent preferably adopts the mixed solvent of one or more in oleyl amine, stearylamine, cetylamine and tetradecy lamine.
In technique scheme, described long-chain fat acid additive preferably adopts one or the mixed solvent of oleic acid or sodium oleate.
In technique scheme, described molybdenum salt preferably adopts ammonium molybdate or Sodium orthomolybdate; Described sulfocompound preferably adopts thiocarbamide or sulphur powder simple substance.
The present invention compared with prior art, have the following advantages and high-lighting effect: the present invention adopts inorganic salt to be raw material, and long-chain amine is solvent as oleyl amine, stearylamine, cetylamine or tetradecy lamine, the molybdenum disulfide nano adopting simple wet chemical method to prepare to have a few atomic is brilliant.Product size is less, good dispersity, the atom number of plies from 1 layer to 5 layers, and well-crystallized.The method of a few atomic molybdenumdisulphide is prepared compared to other, the most important advantage of the method is exactly with low cost, can amplify and carry out industrial production, the method raw material is cheap and easy to get simultaneously, technique is quite simple, and produce and be easy to amplify, product has very outstanding oil soluble, and the ultra-thin molybdenum disulfide nano prepared can directly be scattered in lubricant base, technique is very simple.In a word, the invention provides and a kind ofly synthesize the simple method that alloy has the molybdenum disulfide nano crystalline substance of a few atomic, be very suitable for industrial amplification production, there is very wide application prospect.
Accompanying drawing explanation
Fig. 1 is the x-ray diffractogram of powder that series has the molybdenum disulfide nano crystalline substance of a few atomic.
Fig. 2 is the transmission electron microscope figure of the molybdenum disulfide nano crystalline substance with a few atomic.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described further
A kind of method of synthesizing a few atomic molybdenum disulfide nano crystalline substance provided by the invention, the method is carried out as follows:
1) in long-chain amine solvent, first add long-chain fat acid additive, then add containing molybdenum inorganic salt and sulfocompound, the mol ratio of two kinds of compounds is 0.1 ~ 10:1, and the total mass concentration of two kinds of compounds is generally 0.01 ~ 2.0 gram/ml solvent; Described sulfocompound preferably adopts thiocarbamide or sulphur powder simple substance; Described molybdenum salt preferably adopts ammonium molybdate or Sodium orthomolybdate; Described long-chain amine solvent preferably adopts the mixed solvent of one or more in oleyl amine, stearylamine, cetylamine and tetradecy lamine; Described long-chain fat acid additive preferably adopts one or the mixed solvent of oleic acid or sodium oleate;
2) range of reaction temperature is 160 ~ 300 DEG C, and reaction time range is 30 ~ 120 minutes;
3) by products therefrom washing with alcohol, be scattered in hexanaphthene and preserve, or after drying, directly obtain molybdenum disulfide nano crystalline flour end.
Embodiment 1
Get 10ml oleyl amine and 1ml oleic acid is heated to 160 DEG C, drop into mol ratio is 1:10, total mass is 0.1g ammonium molybdate and thiocarbamide wherein, react 30 minutes, precipitate with washing with alcohol gained after pouring out oleyl amine and oleic acid mixed solvent, dry at 40 DEG C, the ultra-thin molybdenum disulfide nano that can obtain having a few atomic is brilliant.Products obtained therefrom all characterizes with XRD and transmission electron microscope.Its powder x-ray diffraction spectrogram as shown in Figure 1.Its transmission electron microscope photo as shown in Figure 2, the MoS wherein synthesized
2major part is the MoS of 1-5 atomic shell
2nanocrystalline.
Embodiment 2
Get 10ml oleyl amine and 1g sodium oleate is heated to 300 DEG C, drop into mol ratio is 1:5, total mass is 20g ammonium molybdate and thiocarbamide wherein, react 120 minutes, precipitate with washing with alcohol gained after pouring out oleyl amine, dry at 40 DEG C, the ultra-thin molybdenum disulfide nano that can obtain having a few atomic is brilliant.Products obtained therefrom all characterizes with XRD and transmission electron microscope.
Embodiment 3
Get 10ml stearylamine and 5ml oleic acid is heated to 240 DEG C, drop into mol ratio is 5:2, total mass is 5g ammonium molybdate and thiocarbamide wherein, react 60 minutes, precipitate with washing with alcohol gained after pouring out oleyl amine and oleic acid mixed solvent, dry at 40 DEG C, the ultra-thin molybdenum disulfide nano that can obtain having a few atomic is brilliant.Products obtained therefrom all characterizes with XRD and transmission electron microscope.
Embodiment 4
Get 10ml oleyl amine and 10ml oleic acid is heated to 250 DEG C, drop into mol ratio is 1:2, total mass is 2g Sodium orthomolybdate and thiocarbamide wherein, react 30 minutes, precipitate with washing with alcohol gained after pouring out oleyl amine and oleic acid mixed solvent, dry at 40 DEG C, the ultra-thin molybdenum disulfide nano that can obtain having a few atomic is brilliant.Products obtained therefrom all characterizes with XRD and transmission electron microscope.
Embodiment 5
Get 10ml oleyl amine and 1ml oleic acid is heated to 250 DEG C, drop into mol ratio is 1:2, total mass is 0.5g ammonium molybdate and thiocarbamide wherein, react 40 minutes, precipitate with washing with alcohol gained after pouring out oleyl amine and oleic acid mixed solvent, dry at 40 DEG C, the ultra-thin molybdenum disulfide nano that can obtain having a few atomic is brilliant.Products obtained therefrom all characterizes with XRD and transmission electron microscope.
Embodiment 6
Get 10ml oleyl amine and 0.5g sodium oleate is heated to 250 DEG C, drop into mol ratio is 1:2, total mass is 10g ammonium molybdate and thiocarbamide wherein, react 30 minutes, precipitate with washing with alcohol gained after pouring out oleyl amine, dry at 40 DEG C, the ultra-thin molybdenum disulfide nano that can obtain having a few atomic is brilliant.Products obtained therefrom all characterizes with XRD and transmission electron microscope.
Claims (4)
1. synthesize a method for ultra-thin molybdenum disulfide nano crystalline substance, it is characterized in that the method is carried out as follows:
1) in long-chain amine solvent, first add long-chain amine solvent fatty acid additive, then add molybdenum salt and sulfocompound, range of reaction temperature is 160 ~ 300 DEG C, and reaction time range is 30 ~ 120 minutes; The mol ratio of molybdenum salt and sulfocompound is 0.1 ~ 10:1, and both total mass concentrations are 0.01 ~ 2.0 gram/ml;
2) by products therefrom washing with alcohol, be scattered in hexanaphthene and preserve, or after drying, directly obtain molybdenum disulfide nano crystalline flour end.
2. according to a kind of method of synthesizing ultra-thin molybdenum disulfide nano crystalline substance according to claim 1, it is characterized in that: long-chain amine solvent adopts the mixed solvent of one or more in oleyl amine, stearylamine, cetylamine and tetradecy lamine.
3. according to a kind of method of synthesizing ultra-thin molybdenum disulfide nano crystalline substance according to claim 1, it is characterized in that: long-chain fat acid additive adopts one or the mixed solvent of oleic acid or sodium oleate.
4. according to a kind of method of synthesizing ultra-thin molybdenum disulfide nano crystalline substance described in claim 1,2 or 3, it is characterized in that: described molybdenum salt adopts ammonium molybdate or Sodium orthomolybdate; Described sulfocompound adopts thiocarbamide or sulphur powder simple substance.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106893323A (en) * | 2017-03-03 | 2017-06-27 | 江苏大学 | A kind of ultra-thin molybdenum disulfide nano sheet/Self-lubrication composite material of polyimide and preparation method thereof |
| CN108929742A (en) * | 2018-08-31 | 2018-12-04 | 清华大学 | Nano molybdenum disulfide lubricating oil and preparation method thereof |
| CN109110816A (en) * | 2018-10-30 | 2019-01-01 | 中国石油大学(华东) | A kind of synthetic method of oil-soluble molybdenum disulfide |
| CN109943310A (en) * | 2019-04-02 | 2019-06-28 | 侯吉瑞 | A kind of modified MoS2Nano material and preparation method thereof |
| CN110300731A (en) * | 2017-02-02 | 2019-10-01 | 纳米2D材料有限公司 | The 2D stratified material that shines is synthesized using the precursor of amine-metal complex and slow release sulphur |
| CN111378928A (en) * | 2020-04-22 | 2020-07-07 | 中国科学院兰州化学物理研究所 | Nanocrystalline MoS2Solid lubricating film and preparation method and application thereof |
| CN111925668A (en) * | 2020-07-14 | 2020-11-13 | 申雨润滑科技有限公司 | Intercalation inlaid coated oil-soluble molybdenum-based lubricating oil additive and preparation method thereof |
| CN114570937A (en) * | 2022-03-04 | 2022-06-03 | 北京市科学技术研究院分析测试研究所(北京市理化分析测试中心) | Synthesis method of superfine monodisperse nano Ag |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101467893A (en) * | 2007-12-26 | 2009-07-01 | 株式会社东芝 | Ultrasonic diagonstic apparatus, ultrasonic image processing apparatus, and ultrasonic image processing method |
| CN101857265A (en) * | 2010-06-17 | 2010-10-13 | 清华大学 | Method for preparing metal sulfide nanocrystalline |
| CN103915630A (en) * | 2014-04-28 | 2014-07-09 | 华东理工大学 | Molybdenum disulfide/mesoporous carbon composite electrode material as well as preparation method and application thereof |
| CN104030360A (en) * | 2014-07-03 | 2014-09-10 | 中国科学院上海硅酸盐研究所 | Controllable synthesis and synchronous surface modifying method of MoS2 nanosheet |
| CN104108755A (en) * | 2014-07-25 | 2014-10-22 | 深圳新宙邦科技股份有限公司 | Curved-surface molybdenum disulfide nanosheet and preparation method thereof |
| CN104692463A (en) * | 2015-02-15 | 2015-06-10 | 清华大学 | Method for preparing oil-soluble nano-molybdenum disulfide |
-
2015
- 2015-07-20 CN CN201510427922.5A patent/CN105060347B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101467893A (en) * | 2007-12-26 | 2009-07-01 | 株式会社东芝 | Ultrasonic diagonstic apparatus, ultrasonic image processing apparatus, and ultrasonic image processing method |
| CN101857265A (en) * | 2010-06-17 | 2010-10-13 | 清华大学 | Method for preparing metal sulfide nanocrystalline |
| CN103915630A (en) * | 2014-04-28 | 2014-07-09 | 华东理工大学 | Molybdenum disulfide/mesoporous carbon composite electrode material as well as preparation method and application thereof |
| CN104030360A (en) * | 2014-07-03 | 2014-09-10 | 中国科学院上海硅酸盐研究所 | Controllable synthesis and synchronous surface modifying method of MoS2 nanosheet |
| CN104108755A (en) * | 2014-07-25 | 2014-10-22 | 深圳新宙邦科技股份有限公司 | Curved-surface molybdenum disulfide nanosheet and preparation method thereof |
| CN104692463A (en) * | 2015-02-15 | 2015-06-10 | 清华大学 | Method for preparing oil-soluble nano-molybdenum disulfide |
Non-Patent Citations (1)
| Title |
|---|
| CLAUDIA ALTAVILLA, ET AL.: "A Novel Wet Chemistry Approach for the Synthesis of Hybrid 2D Free-Floating Single or Multilayer Nanosheets of MS2@oleylamine(M=Mo,W)", 《CHEMISTRY OF MATERIALS》 * |
Cited By (12)
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| CN110300731A (en) * | 2017-02-02 | 2019-10-01 | 纳米2D材料有限公司 | The 2D stratified material that shines is synthesized using the precursor of amine-metal complex and slow release sulphur |
| CN110300731B (en) * | 2017-02-02 | 2021-11-30 | 纳米2D材料有限公司 | Synthesis of luminescent 2D layered materials using amine-metal complexes and precursors with slow release of sulfur |
| CN106893323A (en) * | 2017-03-03 | 2017-06-27 | 江苏大学 | A kind of ultra-thin molybdenum disulfide nano sheet/Self-lubrication composite material of polyimide and preparation method thereof |
| CN108929742A (en) * | 2018-08-31 | 2018-12-04 | 清华大学 | Nano molybdenum disulfide lubricating oil and preparation method thereof |
| CN108929742B (en) * | 2018-08-31 | 2020-12-15 | 清华大学 | Nano molybdenum disulfide lubricating oil and preparation method thereof |
| CN109110816A (en) * | 2018-10-30 | 2019-01-01 | 中国石油大学(华东) | A kind of synthetic method of oil-soluble molybdenum disulfide |
| CN109943310A (en) * | 2019-04-02 | 2019-06-28 | 侯吉瑞 | A kind of modified MoS2Nano material and preparation method thereof |
| CN109943310B (en) * | 2019-04-02 | 2022-05-24 | 侯吉瑞 | Modified MoS2Nano material and preparation method thereof |
| CN111378928A (en) * | 2020-04-22 | 2020-07-07 | 中国科学院兰州化学物理研究所 | Nanocrystalline MoS2Solid lubricating film and preparation method and application thereof |
| CN111925668A (en) * | 2020-07-14 | 2020-11-13 | 申雨润滑科技有限公司 | Intercalation inlaid coated oil-soluble molybdenum-based lubricating oil additive and preparation method thereof |
| CN114570937A (en) * | 2022-03-04 | 2022-06-03 | 北京市科学技术研究院分析测试研究所(北京市理化分析测试中心) | Synthesis method of superfine monodisperse nano Ag |
| CN114570937B (en) * | 2022-03-04 | 2024-03-29 | 北京市科学技术研究院分析测试研究所(北京市理化分析测试中心) | Synthesis method of superfine monodisperse nano Ag |
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