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Preparation method of monodisperse spherical MoS2 ultrafine powder

An ultra-fine powder, monodisperse technology, applied in the direction of molybdenum sulfide, nanotechnology, etc., can solve the problems of long production process, large impact on subsequent applications, low recovery rate of molybdenum, etc., to achieve good product quality and high utilization rate of raw materials , Engineering zoom in easily effect

Active Publication Date: 2012-08-01
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The molybdenum disulfide product produced by the synthesis method has high purity, and the product with better morphology can be prepared by controlling the reaction process, but in terms of lubricating performance, the molybdenum disulfide of the synthetic lattice is not as good as the molybdenum disulfide of the natural lattice, The main impurities in the product, free sulfur and molybdenum trioxide, have a greater impact on subsequent applications, the production process is longer, the production cost is higher and the recovery rate of molybdenum is lower

Method used

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  • Preparation method of monodisperse spherical MoS2 ultrafine powder
  • Preparation method of monodisperse spherical MoS2 ultrafine powder
  • Preparation method of monodisperse spherical MoS2 ultrafine powder

Examples

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Embodiment 1

[0030] The ammonium tetrathiomolybdate and sulfuric acid are reacted in a ratio of 1:1, (NH 4 ) 2 MoS 4 The concentration of the solution is 0.01mol / L, the concentration of the sulfuric acid solution is 0.05mol / L, no surfactant is added, the stirring rate is 350rpm, the reaction temperature is 20℃, the feed rate is 0.4L / h with a peristaltic pump, and the solution is taken out after 60min of maturation , Separate and wash the solid 3 times, place it in a constant temperature drying oven at 100°C for 2 hours to obtain MoS 3 Of monodisperse particles, figure 2 Monodisperse spherical MoS 3 Scanning electron microscope (SEM) image of. Weigh a certain amount of MoS 3 Place the monodisperse particles in a porcelain boat, put it into the tubular resistance furnace, close the tubular furnace, and inject nitrogen gas at a rate of 0.8L / min for 30 minutes. After replacing the remaining air in the furnace, reduce the nitrogen flow rate to 0.4L / After the furnace body is heated to 800°C, hyd...

Embodiment 2

[0032] The ammonium tetrathiomolybdate and sulfuric acid are reacted in a ratio of 1:1, (NH 4 ) 2 MoS 4 The concentration of the solution is 0.05mol / L, the concentration of the sulfuric acid solution is 10mol / L, the sodium dodecylbenzene sulfonate (DBS) is used as the surfactant, and the amount of surfactant added is the same as the amount of ammonium tetrathiomolybdate The ratio is 0.02:1, the stirring rate is 350rpm, the reaction temperature is 60℃, the feed rate is 0.4L / h with a peristaltic pump, the solution is taken out after 30 minutes of maturation, the solid is separated and washed 3 times, and placed in a constant temperature drying oven at 100℃ Dry for 2h to get MoS 3 Monodisperse particles, weigh a certain amount of MoS 3 Place the monodisperse particles in a porcelain boat, put it into the tubular resistance furnace, close the tubular furnace, and inject nitrogen gas at a rate of 0.8L / min for 30 minutes. After replacing the remaining air in the furnace, reduce the nit...

Embodiment 3

[0034] The ammonium tetrathiomolybdate and nitric acid are reacted at a ratio of 1:0.8, (NH 4 ) 2 MoS 4 The concentration of the solution is 0.01 mol / L, the concentration of the nitric acid solution is 0.05 mol / L, and the cetyl trimethyl ammonium chloride (CTAC) is used as the surfactant. The amount of surfactant added is the same as that of ammonium tetrathiomolybdate. The ratio of the amount of substances is 0.05:1, the stirring rate is 350rpm, the reaction temperature is 0°C, the feed rate of the peristaltic pump is 0.4L / h, the solution is taken out after 5 minutes of maturation, the solid is separated and washed 3 times, and placed in a constant temperature drying box Dry at 100℃ for 2h to get MoS 3 Monodisperse particles, weigh a certain amount of MoS 3 The monodisperse particles, the solids are placed in a porcelain boat, put into the tube-type resistance furnace, the tube-type furnace is sealed, and nitrogen is introduced at a rate of 0.8L / min for 30 minutes. After the res...

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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 [0001] The present invention relates to the field of solid lubricant preparation, in particular, the present invention relates to a monodisperse spherical MoS 2 Preparation method of superfine powder. Background technique [0002] Layered transition metal sulfides (such as MoS 2 ) Has received wide attention due to its special nature. As early as before World War II, MoS 2 It has been widely used as an effective composition of hydrogenation catalysts. Desulfurization from crude oil, namely hydrodesulfurization (HDS), is the most typical example. MoS 2 Another use is closely related to its tribological properties. In MoS 2 Each layer of Mo elements and two layers of S elements are closely packed to form a sandwich-like structure; in the molecular layer, each Mo atom is connected to 6 sulfur atoms, and each sulfur atom is strongly covalently bonded to three Mo atoms. Connection: A crystal formed by stacking and connecting molecular layers and molecular layers throu...

Claims

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Application Information

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IPC IPC(8): C01G39/06B82Y40/00
Inventor 肖清贵陈寅徐红彬张懿
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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