CN102616854A - Preparation method of monodisperse spherical MoS2 ultrafine powder - Google Patents
Preparation method of monodisperse spherical MoS2 ultrafine powder Download PDFInfo
- Publication number
- CN102616854A CN102616854A CN2011100338090A CN201110033809A CN102616854A CN 102616854 A CN102616854 A CN 102616854A CN 2011100338090 A CN2011100338090 A CN 2011100338090A CN 201110033809 A CN201110033809 A CN 201110033809A CN 102616854 A CN102616854 A CN 102616854A
- Authority
- CN
- China
- Prior art keywords
- mos
- monodisperse spherical
- preparation
- superfine powder
- acid
- 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.)
- Granted
Links
Images
Abstract
The invention relates to a preparation method of monodisperse spherical MoS2 ultrafine powder, comprising the following steps: 1) adding a tetrathio ammonium molybdate solution with the concentration of 0.01-0.05 mol/L in a reactor, adding an acid solution dropwisely with the molar ratio of tetrathio ammonium molybdate and acid being 1:0.8-1.5, stirring, reacting, curing, and then carrying out solid-liquid separation, cleaning the solids to obtain monodisperse MoS3 particles; and 2) heating the MoS3 particles obtained in the step 1) under the protection of inert gases, then letting in reducing gases for reacting, cooling to obtain the MoS2 ultrafine powder. According to the invention, (NH4)2MoS4 and the acid solution are used as the raw materials, liquid-phase deposit-hydrogen reduction method is adopted, thus the preparation of the monodisperse spherical MoS2 ultrafine powder is realized, the production conditions are mild, the device requirement is simple, the process flow is short, the utilization rate of raw materials is high, the energy consumption is low, no other impurity is introduced in the production process, the product quality is good, and the purity is high.
Description
Technical field
The present invention relates to the solid lubricant preparation field, particularly, the present invention relates to a kind of monodisperse spherical MoS
2The preparation method of superfine powder.
Background technology
The stratiform transient metal sulfide is (like MoS
2) owing to having special property, it receives extensive concern.Before World War II, MoS
2Use widely with regard to having obtained as effective composition of hydrogenation catalyst, desulfurization is that hydrogenating desulfurization (HDS) is exactly a most typical example from crude oil.MoS
2Another purposes and its tribological property be closely related, at MoS
2In, every layer of Mo element and two-layer S element are through the structure of the similar sandwich of tightly packed formation; In molecular layer, each Mo atom links to each other with 6 sulphur atoms, and each sulphur atom is connected with strong covalent bond with three Mo atoms; The crystal that piles up, is connected to form through Van der Waals force between molecular layer and molecular layer.MoS
2This structure make it have the good lubricity that is similar to graphite, compare other solid lubricants, MoS
2Have high ultimate compression strength and wear resistance, good tack, under high pressure still keep stable film, in most soda acid solvents, all can keep satisfactory stability property; Under high temperature, high rotating speed, high pressure, very low temperature and high vacuum condition, has lubricity efficiently.Therefore, MoS
2The aspect such as bearing lubrication and hydrogenation catalyst that is widely used in industry and aviation field, and MoS
2The preparation of superfine powder then is one of hot issue of solid lubricant area research.Present MoS
2Preparation mainly contain two methods: the one, natural method, with physics or physical chemistry integrated processes to molybdenum glance concentrate purification processing.It is to be raw material with the concentrated molybdenum ore that contains Mo>=57% that natural method is produced molybdenumdisulphide, with acid non-soluble substance, SiO
2, the component that do not have tribology or a lubricity such as Fe (existing with FeS usually) leaches with chemical substance, then separates and removes, dry with far infrared vacuum drying machine again and remove moisture and flotation oil (particularly kerosene and pine camphor oil).Use airflow milling then, being milled to median size like fluidized bed air flow crusher is 1.5～30 μ m, obtains product; The 2nd, synthesis method, synthesis method mainly are divided into wet method sulfuration synthesis method and pyrogenic process sulfuration synthesis method.Wet method sulfuration synthesis method is a raw material with the high-quality molybdenum glance, through oxidizing roasting, ammonia soak, steps such as immersion liquid purification, wet method sulfuration, roasting pyrolysis produce high-purity molybdenumdisulphide; Pyrogenic process sulfuration synthesis method is a raw material with the high-quality molybdenum glance, produces high-purity molybdenumdisulphide through steps such as oxidizing roasting, distillation purification, pyrogenic process sulfuration and pyrolysis.The molybdenumdisulphide product purity of producing through synthesis method is high; And can prepare product with better pattern through the control reaction process; But aspect lubricity, the molybdenumdisulphide of synthetic lattice is not as the molybdenumdisulphide of natural lattice, and major impurity free sulphur in the product and molybdic oxide are bigger to the subsequent applications influence; The technological process of production is longer, and production cost is higher and molybdenum recovery is lower.Compare with first kind of approach, product advantage is more obvious, adopts synthesis method to prepare MoS
2, become one of direction that is worth further investigation.
Summary of the invention
The object of the present invention is to provide a kind of monodisperse spherical MoS
2The preparation method of superfine powder mainly takes liquid-phase precipitation-high-temperature hydrogen reduction two-step approach, realizes monodisperse spherical MoS
2The preparation of superfine powdery material.
According to monodisperse spherical MoS of the present invention
2The preparation method of superfine powder said method comprising the steps of:
1) be the four thio ammonium molybdate solution adding reactor drum of 0.01～0.05mol/L with concentration, drip acid solution, wherein four thio ammonium molybdate is 1: 0.8～1.5 with the mol ratio of acid; Stirring, reaction, slaking; Separate solid-liquid two phases then, clean solid, obtain single MoS of dispersion
3Particle;
2) with step 2) in the MoS that obtains
3Particle is under the protection of rare gas element, and heating feeds the reducing gas reaction again, and cooling obtains monodisperse spherical MoS
2Superfine powder.
According to one embodiment of the invention, monodisperse spherical MoS
2What the preparation method of superfine powder was concrete may further comprise the steps:
1) four thio ammonium molybdate and acid are reacted in the glass reaction still of band heating jacket than 1: 0.8～1.5 ratio in amount of substance, in solution, add proper amount of surfactant or do not add tensio-active agent, (NH
4)
2MoS
4Strength of solution is 0.01～0.05mol/L, and acid solutions is 0.05～10mol/L, and stir speed (S.S.) is 350rpm, and the peristaltic pump feed rate is 0.4L/h; Temperature of reaction is 0～100 ℃, is preferably 20～60 ℃, and the reaction soln curing time is 5～240min; Take out solution, separate solid-liquid two phases, obtain black solid and reaction solution; Deionized water wash gained solid 3 times, and place 100 ℃ of oven dry of thermostatic drying chamber 2h, single MoS that disperses
3Particle;
2) take by weighing single MoS of dispersion in the step 1)
3Particle places porcelain boat, adds in the tube type resistance furnace, and airtight tube furnace is with the speed feeding nitrogen 30min of 0.8L/min; After the trapped air displacement finished in the stove, the reduction nitrogen flow was 0.4L/min, and start program heats up; Treat that body of heater is warming up to 500～800 ℃, the speed with 0.2L/min feeds reducing gas again, insulation 5h; Stop to feed reducing gas and stop the heating, treat that body of heater naturally cools to room temperature after, obtain monodisperse spherical MoS
2Superfine powder.
According to monodisperse spherical MoS of the present invention
2The preparation method of superfine powder, the used acid of said step 1) is one or both in sulfuric acid, nitric acid, hydrochloric acid or the oxalic acid; Said tensio-active agent is X 2073 (DBS), palmityl trimethyl ammonium chloride (CTAC), cetyl trimethylammonium bromide (CTAB), PVP K120 (PVP) and polyoxyethylene glycol (PEG); Said tensio-active agent and four thio ammonium molybdate amount of substance are than 0.02～0.1: 1.
According to monodisperse spherical MoS of the present invention
2The preparation method of superfine powder, said step 2) used reducing gas is a hydrogen.
Monodisperse spherical MoS of the present invention
2The working method of superfine powdery material is by four thio ammonium molybdate ((NH
4)
2MoS
4) produce molybdenumdisulphide (MoS through liquid-phase precipitation-high-temperature hydrogen reduction two-step approach
2), earlier with four thio ammonium molybdate with after acid solution mixes with certain proportion, go out presoma MoS earlier through the liquid-phase precipitation prepared in reaction
3, adopt the high-temperature hydrogen reduction method to obtain MoS again
2Product, principle are to adopt (NH
4)
2MoS
4Solution and acid solution reaction generate MoS
3, generate MoS through high-temperature hydrogen reduction again
2, its reaction formula is following:
(NH
4)
2MoS
4+ 2H
+→ 2NH
4 ++ H
2S+MoS
3↓
Utilize MoS
3The lower characteristic of solubleness in the aqueous solution at first takes the mode of liquid-phase precipitation to produce presoma MoS
3, consider MoS
3Particle diameter is less, and single small-particle has very high surface energy, is easy to reunite generate bigger coacervate, and therefore strict in the present invention control is through control four thio ammonium molybdate ((NH
4)
2MoS
4) concentration, therefore if reunion is very easily sent out in nucleus a large amount of generation, growths of moment because its concentration is too high, be difficult to obtain monodispersed particle, and particle diameter is bigger; If but its concentration is too low, then be difficult for to form nucleus in the solution, after forming nucleus, can on the less nucleus of number, grow, so its particle is often bigger than normal, and homogeneity is difficult to control, therefore with four thio ammonium molybdate ((NH
4)
2MoS
4) concentration be controlled between 0.01～0.05mol/L; And control four thio ammonium molybdate solution and sour mol ratio 1: 0.8～1.5; Under this concentration and proportioning, optimize temperature of reaction, reaction times and and add processing condition such as proper amount of surfactant, control presoma MoS
3Granularity and pattern, make prepared presoma MoS
3Size distribution is narrower, and pattern meets the requirements; With the MoS after the oven dry
3Put into porcelain boat, place in the tube furnace, airtight tube furnace, earlier with air residual in the nitrogen replacement tube furnace, temperature programming feeds reducing gas hydrogen to assigned temperature under nitrogen protection again, obtains monodisperse spherical MoS
2Superfine powder.
The present invention prepares monodisperse spherical MoS
2The superfine powder method was made up of liquid-phase precipitation and two steps of hydrogen reducing.The first step is that four thio ammonium molybdate solution (or adding certain tensio-active agent) makes single amorphous MoS of dispersion through acidifying
3Second step was gained MoS
3At H
2Or H
2/ N
2Make monodisperse spherical MoS through high-temperature hydrogen reduction under the atmosphere
2Superfine powder.Present method is through liquid-phase precipitation regulation and control MoS
3Particle grain size and pattern, thus realize final product MoS
2The regulation and control of grain diameter and pattern.The present invention adopts liquid-phase precipitation-hydrogen reduction two-step approach, under the righttest processing condition, successfully prepares monodisperse spherical MoS
2Superfine powder, this technological operation is convenient, and conversion unit is simple, and engineering is amplified more or less freely.
Produce MoS with prior art
2Technology compare monodisperse spherical MoS provided by the present invention
2The preparation method of superfine powdery material has obvious advantage:
The present invention is with (NH
4)
2MoS
4With acid solution be raw material, adopt liquid-phase precipitation-hydrogen reduction method, realized monodisperse spherical MoS
2The preparation of superfine powdery material, working condition is gentle, and equipment requirements is simple, and technical process is short, and raw material availability is high, and energy consumption is low, does not introduce other impurity in the production process, good product quality, purity is high.
Description of drawings
Fig. 1 is monodisperse spherical MoS of the present invention
2The schematic flow sheet of superfine powdery material generation method;
Fig. 2 is monodisperse spherical MoS among the embodiment 1
3The sem of presoma (SEM) figure;
Fig. 3 is monodisperse spherical MoS among the embodiment 1
2The sem of superfine powder (SEM) figure;
Fig. 4 is monodisperse spherical MoS among the embodiment 1
2The X-ray diffraction of superfine powder (XRD) collection of illustrative plates;
Fig. 5 is monodisperse spherical MoS among the embodiment 1
2(EDS) collection of illustrative plates of superfine powder;
Fig. 6 is monodisperse spherical MoS among the embodiment 2
2The sem of superfine powder (SEM) figure;
Fig. 7 is monodisperse spherical MoS among the embodiment 3
2The sem of superfine powder (SEM) figure;
Fig. 8 is monodisperse spherical MoS among the embodiment 4
2The sem of superfine powder (SEM) figure;
Fig. 9 is monodisperse spherical MoS among the embodiment 5
2The sem of superfine powder (SEM) figure;
Figure 10 is monodisperse spherical MoS among the embodiment 6
2The sem of superfine powder (SEM) figure.
Embodiment
Embodiment 1
Four thio ammonium molybdate and sulfuric acid are reacted (NH than 1: 1 ratio in amount of substance
4)
2MoS
4Strength of solution is 0.01mol/L, and sulphuric acid soln concentration is 0.05mol/L, does not add tensio-active agent; Stir speed (S.S.) is 350rpm, and temperature of reaction is 20 ℃, uses the peristaltic pump feed rate to be 0.4L/h; Take out solution behind the slaking 60min; Separation and wash solids 3 times place 100 ℃ of oven dry of thermostatic drying chamber 2h, obtain MoS
3Monodisperse particles, Fig. 2 is monodisperse spherical MoS
3Sem (SEM) figure.Take by weighing a certain amount of gained MoS
3Monodisperse particles place porcelain boat, add in the tube type resistance furnace, airtight tube furnace feeds nitrogen 30min with the speed of 0.8L/min; After the trapped air displacement finished in the stove, the reduction nitrogen flow was 0.4L/min, and start program heats up; Treat that body of heater is warming up to 800 ℃, the speed with 0.2L/min feeds hydrogen again, behind the insulation 5h; Stop to feed hydrogen and stop the heating, treat that body of heater naturally cools to room temperature after, obtain monodisperse spherical MoS
2Particle, its particle median size is 450nm, Fig. 3 is the monodisperse spherical MoS for preparing
2The sem of superfine powder (SEM) figure; Fig. 4 is the monodisperse spherical MoS for preparing
2The X-ray diffraction of superfine powder (XRD) collection of illustrative plates; Fig. 5 is the monodisperse spherical MoS for preparing
2(EDS) collection of illustrative plates of superfine powder.
Embodiment 2
Four thio ammonium molybdate and sulfuric acid are reacted (NH than 1: 1 ratio in amount of substance
4)
2MoS
4Strength of solution is 0.05mol/L, and sulphuric acid soln concentration is 10mol/L, is tensio-active agent with X 2073 (DBS); The add-on of tensio-active agent is 0.02: 1 with the ratio of the amount of substance of four thio ammonium molybdate, and stir speed (S.S.) is 350rpm, and temperature of reaction is 60 ℃; Use the peristaltic pump feed rate to be 0.4L/h, take out solution behind the slaking 30min, separation and wash solids 3 times; Place 100 ℃ of oven dry of thermostatic drying chamber 2h, obtain MoS
3Monodisperse particles, take by weighing a certain amount of gained MoS
3Monodisperse particles place porcelain boat, add in the tube type resistance furnace, airtight tube furnace feeds nitrogen 30min with the speed of 0.8L/min; After the trapped air displacement finished in the stove, the reduction nitrogen flow was 0.4L/min, and start program heats up; Treat that body of heater is warming up to 750 ℃, the speed with 0.2L/min feeds hydrogen again, behind the insulation 5h; Stop to feed hydrogen and stop the heating, treat that body of heater naturally cools to room temperature after, obtain monodisperse spherical MoS
2Particle, average particle size are 200nm, and Fig. 6 is the monodisperse spherical MoS for preparing
2The sem of superfine powder (SEM) figure.
Embodiment 3
Four thio ammonium molybdate and nitric acid are reacted (NH than 1: 0.8 ratio in amount of substance
4)
2MoS
4Strength of solution is 0.01mol/L, and salpeter solution concentration is 0.05mol/L, is tensio-active agent with palmityl trimethyl ammonium chloride (CTAC); The add-on of tensio-active agent is 0.05: 1 with the ratio of the amount of substance of four thio ammonium molybdate, and stir speed (S.S.) is 350rpm, and temperature of reaction is 0 ℃; The peristaltic pump feed rate is 0.4L/h, takes out solution behind the slaking 5min, separation and wash solids 3 times; Place 100 ℃ of oven dry of thermostatic drying chamber 2h, obtain MoS
3Monodisperse particles, take by weighing a certain amount of MoS
3Monodisperse particles, solid places porcelain boat, adds in the tube type resistance furnace airtight tube furnace; Speed with 0.8L/min feeds nitrogen 30min, and after the trapped air displacement finished in the stove, the reduction nitrogen flow was 0.4L/min, and start program heats up; Treat that body of heater is warming up to 650 ℃, the speed with 0.2L/min feeds hydrogen again, behind the insulation 5h; Stop to feed hydrogen and stop the heating, treat that body of heater naturally cools to room temperature after, obtain monodisperse spherical MoS
2Particle, average particle size are 500nm, and Fig. 7 is the monodisperse spherical MoS for preparing
2The sem of superfine powder (SEM) figure.
Four thio ammonium molybdate and hydrochloric acid are reacted (NH than 1: 1.2 ratio in amount of substance
4)
2MoS
4Strength of solution is 0.05mol/L, and concentration of hydrochloric acid solution is 5mol/L, is tensio-active agent with cetyl trimethylammonium bromide (CTAB); The add-on of tensio-active agent is 0.08: 1 with the ratio of the amount of substance of four thio ammonium molybdate, and stir speed (S.S.) is 350rpm, and temperature of reaction is 100 ℃; Use the peristaltic pump feed rate to be 0.4L/h, take out solution behind the slaking 240min, separation and wash solids 3 times; Place 100 ℃ of oven dry of thermostatic drying chamber 2h, obtain MoS
3Monodisperse particles, take by weighing a certain amount of MoS
3Monodisperse particles, place porcelain boat, add in the tube type resistance furnace airtight tube furnace; Speed with 0.8L/min feeds nitrogen 30min, and after the trapped air displacement finished in the stove, the reduction nitrogen flow was 0.4L/min, and start program heats up; Treat that body of heater is warming up to 500 ℃, the speed with 0.2L/min feeds hydrogen again, behind the insulation 5h; Stop to feed hydrogen and stop the heating, treat that body of heater naturally cools to room temperature after, obtain monodisperse spherical MoS
2Particle, average particle size are 400nm, and Fig. 8 is the monodisperse spherical MoS for preparing
2The sem of superfine powder (SEM) figure.
Embodiment 5
Four thio ammonium molybdate and oxalic acid are reacted (NH than 1: 1.5 ratio in amount of substance
4)
2MoS
4Strength of solution is 0.05mol/L, and oxalic acid solution concentration is 1mol/L, is tensio-active agent with PVP K120 (PVP); The add-on of tensio-active agent is 0.1: 1 with the ratio of the amount of substance of four thio ammonium molybdate, and stir speed (S.S.) is 350rpm, and temperature of reaction is 80 ℃; Use the peristaltic pump feed rate to be 0.4L/h, take out solution behind the slaking 60min, separation and wash solids 3 times; Place 100 ℃ of oven dry of thermostatic drying chamber 2h, obtain MoS
3Monodisperse particles, take by weighing a certain amount of MoS
3Monodisperse particles, place porcelain boat, add in the tube type resistance furnace airtight tube furnace; Speed with 0.8L/min feeds nitrogen 30min, and after the trapped air displacement finished in the stove, the reduction nitrogen flow was 0.4L/min, and start program heats up; Treat that body of heater is warming up to 800 ℃, the speed with 0.2L/min feeds hydrogen again, behind the insulation 5h; Stop to feed hydrogen and stop the heating, treat that body of heater naturally cools to room temperature after, obtain monodisperse spherical MoS
2Particle, average particle size are 250nm, and Fig. 9 is the monodisperse spherical MoS for preparing
2The sem of superfine powder (SEM) figure.
Embodiment 6
Four thio ammonium molybdate and hydrochloric acid, sulfuric acid nitration mixture are reacted (NH than 1: 0.5: 0.5 ratio in amount of substance
4)
2MoS
4Strength of solution is 0.05mol/L, and hydrochloric acid, sulphuric acid soln concentration are 5mol/L, is tensio-active agent with polyoxyethylene glycol (PEG); The add-on of tensio-active agent is 0.03: 1 with the ratio of the amount of substance of four thio ammonium molybdate, and stir speed (S.S.) is 350rpm, and temperature of reaction is 55 ℃; Use the peristaltic pump feed rate to be 0.4L/h, take out solution behind the slaking 60min, separation and wash solids 3 times; Place 100 ℃ of oven dry of thermostatic drying chamber 2h, obtain MoS
3Monodisperse particles, take by weighing a certain amount of MoS
3Monodisperse particles, place porcelain boat, add in the tube type resistance furnace airtight tube furnace; Speed with 0.8L/min feeds nitrogen 30min, and after the trapped air displacement finished in the stove, the reduction nitrogen flow was 0.4L/min, and start program heats up; Treat that body of heater is warming up to 800 ℃, the speed with 0.2L/min feeds hydrogen again, behind the insulation 5h; Stop to feed hydrogen and stop the heating, treat that body of heater naturally cools to room temperature after, obtain monodisperse spherical MoS
2Particle, average particle size are 350nm, and Figure 10 is the monodisperse spherical MoS for preparing
2The sem of superfine powder (SEM) figure.
Claims (6)
1. according to the said monodisperse spherical MoS of claim 1
2The preparation method of superfine powder is characterized in that, said method comprising the steps of:
1) be the four thio ammonium molybdate solution adding reactor drum of 0.01～0.05mol/L with concentration, drip acid solution, wherein four thio ammonium molybdate is 1: 0.8～1.5 with the mol ratio of acid; Stirring, reaction, slaking; Separate solid-liquid two phases then, clean solid, obtain single MoS of dispersion
3Particle;
2) with the MoS that obtains in the step 1)
3Particle is under the protection of rare gas element, and heating feeds the reducing gas reaction again, and cooling obtains monodisperse spherical MoS
2Superfine powder.
2. according to the said monodisperse spherical MoS of claim 1
2The preparation method of superfine powder; It is characterized in that; In said step 1), add tensio-active agent; Said tensio-active agent is X 2073, palmityl trimethyl ammonium chloride, cetyl trimethylammonium bromide, PVP K120 or polyoxyethylene glycol, and the tensio-active agent of adding is 0.02～0.1: 1 with the amount of substance of four thio ammonium molybdate ratio.
3. according to the said monodisperse spherical MoS of claim 1
2The preparation method of superfine powder is characterized in that, acid solution is one or both in sulfuric acid, nitric acid, hydrochloric acid or the oxalic acid in the said step 1).
4. according to the said monodisperse spherical MoS of claim 1
2The preparation method of superfine powder is characterized in that, the acid droplet rate of acceleration is 0.4L/h in the said step 1), and stir speed (S.S.) is 350rpm, and temperature of reaction is 0～100 ℃, and the curing time is 5～240min.
5. according to the said monodisperse spherical MoS of claim 4
2The preparation method of superfine powder is characterized in that, said step 1) temperature of reaction is 20～60 ℃,
6. according to the said monodisperse spherical MoS of claim 1
2The preparation method of superfine powder is characterized in that, in said step 2) in; Said rare gas element is a nitrogen, and aeration time is 30min, under protection of inert gas, is heated to 500～800 ℃; Feed reducing gas, said reducing gas is a hydrogen, and Ventilation Rate is 0.2L/min; Carry out reduction reaction, the reaction times is 5h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110033809.0A CN102616854B (en) | 2011-01-31 | 2011-01-31 | Preparation method of monodisperse spherical MoS2 ultrafine powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110033809.0A CN102616854B (en) | 2011-01-31 | 2011-01-31 | Preparation method of monodisperse spherical MoS2 ultrafine powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102616854A true CN102616854A (en) | 2012-08-01 |
| CN102616854B CN102616854B (en) | 2014-11-05 |
Family
ID=46557140
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110033809.0A Active CN102616854B (en) | 2011-01-31 | 2011-01-31 | Preparation method of monodisperse spherical MoS2 ultrafine powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102616854B (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103143373A (en) * | 2013-03-13 | 2013-06-12 | 南开大学 | Method for preparing hydrodesulfurization catalyst |
| CN103693693A (en) * | 2013-12-26 | 2014-04-02 | 湛江师范学院 | Preparation method for synthesizing molybdenum sulfide nanospheres by microwave-assisted liquid phase deposition |
| CN104674025A (en) * | 2013-11-28 | 2015-06-03 | 韩国地质资源研究院 | Method of pre-treating molybdenite containing copper |
| CN104707629A (en) * | 2015-04-08 | 2015-06-17 | 兰州理工大学 | Preparation method of hydrogenating catalyst for load type transition metal sulfide |
| CN105347401A (en) * | 2015-11-19 | 2016-02-24 | 常州大学 | Method used for controllable preparation of monodisperse mesoporous molybdenum disulfide nanospheres |
| CN110508294A (en) * | 2018-05-21 | 2019-11-29 | 中国石油化工股份有限公司 | Hydrogenation catalyst preparation method and by this method preparation hydrogenation catalyst and application |
| CN113461061A (en) * | 2021-07-28 | 2021-10-01 | 洛阳申雨钼业有限责任公司 | Preparation method of high-purity molybdenum disulfide |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1752023A (en) * | 2005-08-11 | 2006-03-29 | 上海交通大学 | Preparation method of inorganic fullerene structured molybdenium disulfide |
| CN101857273A (en) * | 2010-05-26 | 2010-10-13 | 上海大学 | Preparation method of nanoscale flaky molybdenum disulfide |
-
2011
- 2011-01-31 CN CN201110033809.0A patent/CN102616854B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1752023A (en) * | 2005-08-11 | 2006-03-29 | 上海交通大学 | Preparation method of inorganic fullerene structured molybdenium disulfide |
| CN101857273A (en) * | 2010-05-26 | 2010-10-13 | 上海大学 | Preparation method of nanoscale flaky molybdenum disulfide |
Non-Patent Citations (3)
| Title |
|---|
| DU, KAI等: "Synthesis of inorganic fullerene-like MoS2 nanoparticles by a facile method", 《MATERIALS LETTERS》 * |
| 徐志昌等: "MoS2纳米材料化学合成工艺流程的研究", 《中国钼业》 * |
| 邹同征等: "聚乙二醇为分散剂的沉淀法制备IF-MoS2", 《无机化学学报》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103143373A (en) * | 2013-03-13 | 2013-06-12 | 南开大学 | Method for preparing hydrodesulfurization catalyst |
| CN104674025A (en) * | 2013-11-28 | 2015-06-03 | 韩国地质资源研究院 | Method of pre-treating molybdenite containing copper |
| CN103693693A (en) * | 2013-12-26 | 2014-04-02 | 湛江师范学院 | Preparation method for synthesizing molybdenum sulfide nanospheres by microwave-assisted liquid phase deposition |
| CN104707629A (en) * | 2015-04-08 | 2015-06-17 | 兰州理工大学 | Preparation method of hydrogenating catalyst for load type transition metal sulfide |
| CN105347401A (en) * | 2015-11-19 | 2016-02-24 | 常州大学 | Method used for controllable preparation of monodisperse mesoporous molybdenum disulfide nanospheres |
| CN110508294A (en) * | 2018-05-21 | 2019-11-29 | 中国石油化工股份有限公司 | Hydrogenation catalyst preparation method and by this method preparation hydrogenation catalyst and application |
| CN113461061A (en) * | 2021-07-28 | 2021-10-01 | 洛阳申雨钼业有限责任公司 | Preparation method of high-purity molybdenum disulfide |
| CN113461061B (en) * | 2021-07-28 | 2022-08-23 | 洛阳申雨钼业有限责任公司 | Preparation method of high-purity molybdenum disulfide |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102616854B (en) | 2014-11-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102616854B (en) | Preparation method of monodisperse spherical MoS2 ultrafine powder | |
| Ibarguen et al. | Synthesis of SnO2 nanoparticles through the controlled precipitation route | |
| WO2010037709A2 (en) | Production of solar-grade silicon from silicon dioxide | |
| CN111187958B (en) | Mo powder/MoO2Method for preparing nano lanthanum-molybdenum oxide alloy by doping with lanthanum ammonium molybdate powder | |
| CN106994517B (en) | A kind of preparation method of high-thermal-conductivity low-expansibility W-Cu encapsulating material | |
| CN108565434B (en) | Preparation method of tungsten disulfide/nitrogen and sulfur co-doped graphene compound | |
| CN101979443A (en) | Method for producing modified white carbon black | |
| CN105256146A (en) | Method for recycling metal palladium from waste palladium-aluminum oxide catalysts | |
| EP3206989A1 (en) | Method for producing silicon by means of magnesiothermal reduction | |
| CN103626191A (en) | Preparation method of nano-scale silicon dioxide | |
| Asadi et al. | Optimization of colloidal nanosilica production from expanded perlite using Taguchi design of experiments | |
| CN104418332B (en) | A kind of preparation method of silicon dioxide | |
| CN103302300A (en) | Preparation method of tungsten nano powder | |
| CN106041111B (en) | The method that a kind of ammonium paratungstate or ammonium metatungstate containing arsenic and phosphorus prepare nano-tungsten powder | |
| CN104944475A (en) | Preparation method of cobalt carbonate with super coarse particles and high purity | |
| CN105621485A (en) | Preparation method of vanadium trioxide powder | |
| CN109019690B (en) | Short-process preparation method of rare earth doped modified ammonium paratungstate powder | |
| Ye et al. | Microemulsion-assisted hydrothermal preparation and infrared radiation property of TiO2 nanomaterials with tunable morphologies and crystal form | |
| CN102717070A (en) | Method for preparing carbon-coated copper nano particles through liquid alkane reflux method | |
| JP5315614B2 (en) | Pretreatment method of nickel oxide ore | |
| Tao et al. | Synthesis and growth mechanism of monodispersed MoS 2 sheets/carbon microspheres | |
| Tsai | Formation of nanocrystalline cerium oxide and crystal growth | |
| CN105154169A (en) | Tungsten disulfide/molybdenum disulfide/montmorillonite compound and preparation method thereof | |
| CN110983091B (en) | Method for preparing nano tungsten-based powder material by doping yttrium oxide in liquid-liquid manner | |
| CN103303979B (en) | Tungsten oxide (WO3) nanopowder prepared by pyrolysing method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |