CN102603006A - Method for synthetizing nanometer molybdenum disulfide transparent colloid - Google Patents
Method for synthetizing nanometer molybdenum disulfide transparent colloid Download PDFInfo
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- CN102603006A CN102603006A CN2011104287844A CN201110428784A CN102603006A CN 102603006 A CN102603006 A CN 102603006A CN 2011104287844 A CN2011104287844 A CN 2011104287844A CN 201110428784 A CN201110428784 A CN 201110428784A CN 102603006 A CN102603006 A CN 102603006A
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Abstract
The invention relates to a method for synthetizing nanometer molybdenum disulfide transparent colloid. In the method, ammonium molybdate tetrahydrate is used as a molybdenum source, thiourea is used as a sulphur source and a reductant, in a solvent having a specific proportion, the nanometer molybdenum disulfide colloid is directly prepared by adopting a solvothermal method under a certain reaction condition, thereby improving the dispersity of the colloid in organic solvents. According to the invention, the nanometer colloid is synthetized by utilizing the direct solvothermal method of a mixed solvent, so as to ensure that nanometer molybdenum disulfide is uniformly dispersed in ethanol so that stable colloid of which the Zeta potential is 11.4 is formed. The method disclosed by the invention is simple in process, low in cost and short in synthesis time and has high application value.
Description
Technical field
The present invention relates to a kind of molybdenumdisulphide self-lubricating colloidal compound method, belong to nano material preparation and dispersion technology field.
Background technology
Molybdenumdisulphide is the pressed powder of a kind of pewter to black, has metalluster, and good chemicalstability and thermostability have been touched soapy feeling, is applicable to lubricated field.Compare with common molybdenumdisulphide; Nano molybdenum disulfide is further improved on the performance in every respect; Caused in recent years widely and paid close attention to that show several aspects highlightedly: the frictional coefficient of micron order molybdenumdisulphide was between 0.03 ~ 0.06, and ys reaches 352kg/mm
2, in-190 ~ 300 ℃ of scopes, show effectively lubricating.And the nano molybdenum disulfide fineness is lower, and specific surface area is bigger, and the concave point ability at packing lubrication interface is stronger; Tack and level of coverage in friction material surface all obviously improve; Frictional coefficient is lower, and frictional coefficient is generally 0.008 ~ 0.01, and anti-attrition property is very excellent; The nano molybdenum disulfide thin layer can be with nearly 1178 eV of differential, be complementary with the energy of light, on the sensitive cell material, application prospect is arranged; After what is interesting is that more the molybdenumdisulphide interlayer inserts organic group, can form the two-dimensional nano mixture, these mixtures be not simply adding of inorganics character and matter property and, but show the characteristic of many excellences.
The main pattern of nano molybdenum disulfide comprises nanoparticle, nano thin-layer, nano-complex, soccerballene shape nanoparticle and nanotube etc.Main preparation methods has methods such as the precipitator method, solvent-thermal method, precursor pyrolytic decomposition, electrochemistry.Wherein solvent-thermal method synthetic nano-powder has that the reunion degree is light, purity is high, narrow diameter distribution, form are controlled, crystal grain component and crystal grain are grown advantages such as complete.
But because the surface energy of nano particle is big, reunite easily, be difficult for stable dispersion in solution, if the various performances of the nano molybdenum disulfide of bringing into play must solve its scattering problem.People have done a lot of work through the surface modification treatment material to improve its applicability, for nano-powder, on the one hand: on the one hand; The surface chemistry of control nano-powder is formed; Improving its Surface Physical Chemistry performance, is to expand nano-powder to use, and improves the key of its added value; On the other hand, the nano-powder particle surface energy is high, is prone to reunite, and therefore, changes the wettability of powder, and improving the dispersion behavior of nano-powder in solution system or polymeric matrix also is one of important application of surface-treated.
Single molybdenum disulfide nano particulate can not form stable colloidal solutions with lubricating oil, even use surfactant-modified nano-powder, effect is also also not obvious.It is initiator that people such as Hu Xianguo utilize Diisopropyl azodicarboxylate (AIBN), and Vinylpyrrolidone polymer (PVP) is a dispersion agent, and modified Nano molybdenumdisulphide powder is dispersed in powder in the Oil solvent, forms stable oily liquids.People such as Guo Qiang design and have synthesized a kind of organic-molybdenum compound coupling agent, and with it molybdenumdisulphide are carried out surface-treated, and the nano-powder after the modification is soluble in organic resin solution, has obviously improved its dispersiveness.Its method is comparatively complicated, and cost is higher.If but the purpose of corresponding tensio-active agent or dispersion agent only is to make molybdenumdisulphide powder and the affine formation homogeneous latex emulsion of organic solvent, too complicated multiple additives composition constitutes unfavorable factor for the lubricity that improves additive, maintenance additive stability.
Summary of the invention
The purpose of this invention is to provide the method that a kind of solvent-thermal method prepares the nano molybdenum disulfide transparent colloid.
The object of the invention can be realized in the following manner:
With Ammonium Molybdate Tetrahydrate and thiocarbamide is feedstock production molybdenumdisulphide colloid; May further comprise the steps:
incorporates Ammonium Molybdate Tetrahydrate and thiocarbamide in a certain amount of deionized water by a certain percentage, and ultrasonic dissolution;
joins adequate amount of ethanol and N-Methyl pyrrolidone in the aqueous solution, stirs;
places reaction kettle with the reaction soln that configures, according to certain reaction conditions and time insulation reaction;
reaction finishes postcooling to room temperature, and reaction solution is added deionized water precipitin reaction product;
is through post precipitation; The upper strata stillness of night is removed; Add alcohol solvent, form the nano molybdenum disulfide colloid.
Condition is that Ammonium Molybdate Tetrahydrate and thiocarbamide are according to 10: 9 mixed of mass ratio among the said preparation technology; Deionized water and alcoholic acid volume ratio are 3: 1～4:1; The volume ratio of ethanol and N-Methyl pyrrolidone is 1:1～1:2; Temperature of reaction is 180 oC～200 oC, and the reaction times is 3h～8h.
The present invention has the following advantages:
(1) the present invention utilizes mixed solvent, adopts solvent-thermal method directly to prepare nano molybdenum disulfide colloid (like Fig. 1), demonstrates tangible Tyndall phenomenon.Gained colloidal particle (like Fig. 2) even particle size, good dispersibility.
(2) colloidal stability of the present invention's preparation is good, and the Zeta current potential has good dispersiveness up to 11.4 in organic matrix (comprising lubricating oil, resin etc.).
(3) the present invention makes the nanometer colloid of good dispersibility one step, has improved its using value in organic matrix greatly.
(4) technological process of the present invention is simple, with low cost, with short production cycle, has very high using value.
Description of drawings
Fig. 1 prepares molybdenumdisulphide colloidal Tyndall phenomenon for the present invention.
Fig. 2 prepares molybdenumdisulphide colloidal TEM photo for the present invention.
Embodiment
Embodiment 1
Analytically pure Ammonium Molybdate Tetrahydrate and thiocarbamide are joined in the deionized water of 30 mL according to 10: 9 ratio of mass ratio, stir and ultrasonic decomposition, make its dissolving.According to the volume ratio of ethanol and N-Methyl pyrrolidone is that the ratio of 1:1～1:2 adds ethanol and N-Methyl pyrrolidone in the aqueous solution, stirs and ultrasonic, and it is mixed, and this moment, solution was blue.The solution that configures inserted in the reaction kettle seal, then reaction kettle is placed the baking oven of 180 oC～200 oC, reaction 3～6 h.Question response is cooled to room temperature after finishing, and reaction solution is used washed with de-ionized water, deposition.Post precipitation is removed upper solution, adds ethanol then and just obtains the nano molybdenum disulfide colloid.Through test, the uniform particles of its colloidal particle.The Zeta current potential is 4.9.
Embodiment 2
Analytically pure Ammonium Molybdate Tetrahydrate and thiocarbamide are joined in the deionized water of 40 mL according to 10: 9 ratio of mass ratio, stir and ultrasonic decomposition, make its dissolving.According to the volume ratio of ethanol and N-Methyl pyrrolidone is that the ratio of 1:1～1:2 adds ethanol and N-Methyl pyrrolidone in the aqueous solution, stirs and ultrasonic, and it is mixed, and this moment, solution was blue.The solution that configures inserted in the reaction kettle seal, then reaction kettle is placed the baking oven of 180 oC～200 oC, reaction 3～6 h.Question response is cooled to room temperature after finishing, and reaction solution is used washed with de-ionized water, deposition.Post precipitation is removed upper solution, adds ethanol then and just obtains the nano molybdenum disulfide colloid.Through test, the uniform particles of its colloidal particle.The Zeta current potential is 11.4.
Claims (4)
1. the compound method of a nano molybdenum disulfide transparent colloid; With Ammonium Molybdate Tetrahydrate and thiocarbamide is feedstock production molybdenumdisulphide colloid; It is characterized in that may further comprise the steps:
incorporates Ammonium Molybdate Tetrahydrate and thiocarbamide in a certain amount of deionized water by a certain percentage, and ultrasonic dissolution;
joins adequate amount of ethanol and N-Methyl pyrrolidone in the aqueous solution; Form mixed solvent, stir;
places reaction kettle with the reaction soln that configures, according to certain reaction conditions and time insulation reaction;
reaction finishes postcooling to room temperature, and reaction solution is added deionized water precipitin reaction product;
is through post precipitation; Supernatant liquid is removed; Add alcohol solvent, form the nano molybdenum disulfide colloid.
2. the compound method of nano molybdenum disulfide transparent colloid as claimed in claim 1 is characterized in that: the mass ratio of Ammonium Molybdate Tetrahydrate and thiocarbamide is 10: 9 in the said step
.
3. the compound method of nano molybdenum disulfide transparent colloid as claimed in claim 1; It is characterized in that: the volume ratio that adds ethanol and deionized water in the said step
is 1:3～1:4, and the volume ratio of ethanol and N-Methyl pyrrolidone is 1: 1～1: 2.
4. the compound method of nano molybdenum disulfide transparent colloid as claimed in claim 1 is characterized in that: reaction conditions is that 180 ℃～200 ℃ of temperature of reaction, reaction times are 3～8 h in the said step
.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104689836A (en) * | 2013-12-04 | 2015-06-10 | 中国科学院大连化学物理研究所 | Highly dispersed nano molybdenum disulfide catalyst synthetic method |
| CN111960468A (en) * | 2020-08-21 | 2020-11-20 | 中国科学院宁波材料技术与工程研究所 | Two-dimensional transition metal chalcogenide wave-absorbing material, preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2030468C1 (en) * | 1991-11-18 | 1995-03-10 | Приаргунское производственное горно-химическое объединение | Method of molybdenum disulfide producing |
| CN1994895A (en) * | 2006-12-20 | 2007-07-11 | 浙江大学 | Preparation method for ion liquid assisted hydrothermal synthesis of MoS2 microsphere |
| CN101851006A (en) * | 2010-06-08 | 2010-10-06 | 南开大学 | Method for preparing MoS2 microspheres by solvent hot method |
-
2011
- 2011-12-20 CN CN2011104287844A patent/CN102603006A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2030468C1 (en) * | 1991-11-18 | 1995-03-10 | Приаргунское производственное горно-химическое объединение | Method of molybdenum disulfide producing |
| CN1994895A (en) * | 2006-12-20 | 2007-07-11 | 浙江大学 | Preparation method for ion liquid assisted hydrothermal synthesis of MoS2 microsphere |
| CN101851006A (en) * | 2010-06-08 | 2010-10-06 | 南开大学 | Method for preparing MoS2 microspheres by solvent hot method |
Non-Patent Citations (1)
| Title |
|---|
| "液相化学法合成纳米二硫化钼研究进展": "王泉山等", 《广东化工》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104689836A (en) * | 2013-12-04 | 2015-06-10 | 中国科学院大连化学物理研究所 | Highly dispersed nano molybdenum disulfide catalyst synthetic method |
| CN111960468A (en) * | 2020-08-21 | 2020-11-20 | 中国科学院宁波材料技术与工程研究所 | Two-dimensional transition metal chalcogenide wave-absorbing material, preparation method and application thereof |
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Application publication date: 20120725 |