CN109867305A - A kind of preparation method of nano molybdenum disulfide - Google Patents

Abstract

A kind of preparation method of nano molybdenum disulfide, the method comprises the following steps: the mass ratio of a, configuration intercalant solution, intercalator and deionized water is 1:0.8-10；B, molybdenum disulfide is fitted into three mouthfuls of closed containers, by container vacuum-pumping, vacuum degree control is in 1.3-60Kpa；The intercalant solution of preparation is sucked in container by a mouth of closed container, soakage, which all floods molybdenum disulfide solid with intercalant solution, to be advisable, and opens closed container drain and releases vacuum, restore normal pressure, controls immersion 10-24 hours of 20-80 DEG C of temperature；C, slurries filtering is impregnated, obtained solid molybdenum disulfide after filtering is washed using deionized water then, is dried in vacuo under conditions of 40-60 DEG C of drying temperature later, drying time 2-12 hour；D, the dried molybdenum disulfide containing intercalator is put into micro-wave oven, regulation power 100-180KW, is held time 5-60 minutes, nano molybdenum disulfide powder can be obtained using wet classification technology later.

Description

A kind of preparation method of nano molybdenum disulfide

Technical field

The present invention relates to a kind of molybdenum disulfide preparation technical fields, more particularly to a kind of preparation side of nano molybdenum disulfide Method.

Background technique

Molybdenum disulfide is important solid lubricant, in the environment of high temperature, high pressure, low temperature, high vacuum.It Also there is diamagnetism, can be used as linear photoconductor conductor and show the semiconductor of p-type or N-type conductivity energy, there is rectification and transducing Effect.Molybdenum disulfide also acts as the catalyst of complicated dehydrogenation of hydrocarbons.

Molybdenum disulfide is known as " advanced solid lubricant king ", molybdenum disulfide be by natural molybdenum concentrate powder after chemical purification Manufactured solid powder；The black slightly band silver gray of this product color, there is metallic luster, and touching has a soapy feeling, not soluble in water.Product, which has, to be divided Scattered property is good, and inadherent advantage can add in various greases, forms inadherent colloidal state absolutely, can increase the profit of grease Slip and extreme pressure property；It is also applied for the machine work state of high temperature, high pressure, high revolving speed high load capacity, extends equipment life.

Existing preparation nanometer MoS₂The method of material, can be mainly divided into two major classes: physical method and chemical method.Physics Method mainly includes: common molybdenum disulfide is mechanically pulverized staging, physical vaporous deposition (PVD), micromechanical forces stripping method and Liquid phase stripping method etc..Chemical method is main are as follows: hydro-thermal method, chemical vapour deposition technique (CVD), vulcanization, electrochemical deposition method etc.. But these methods have the disadvantage that preparation process energy consumption height, low yield, at high cost, not environmentally, seriously hinder MoS₂Material It is extensive, produce in enormous quantities, it is limited so as to cause its application range.

Chinese patent application CN108640154A discloses a kind of molybdenum disulfide nano material and preparation method thereof, the patent Application uses ionic liquid for electrolyte, prepares nano molybdenum disulfide, but ionic liquid price using curing molybdenum bar electrolysis method Height, electrolytic condition is harsh, and last handling process is cumbersome, is unfavorable for large-scale production.Chinese patent application CN108862387A is disclosed A kind of preparation method of anisotropic nano molybdenum disulfide, it is carrier that this method, which first uses many oxide nano particle, with molybdic acid Ammonium is molybdenum forerunner species oxide impregnation object carrier, and support type curing molybdenum materials is made under specific conditions of vulcanization after drying, roasting Material finally removes oxide carrier with hydrofluoric acid chemical etching, several nanometers of special-shaped nanoscales to tens nanometer ranges can be obtained Molybdenum disulfide material, at high cost, the hydrofluoric acid seriously corroded used, harm to the human body are big.

Summary of the invention

The purpose of the present invention is exactly the shortcoming being directed in the presence of the above-mentioned prior art and provides a kind of low cost, big Scale prepares the preparation method of nano molybdenum disulfide.Method of the invention is inserted into two using intercalation-microexplosion Hong technology, by intercalator The interlayer of molybdenum sulfide, then ignited by microwave, make micro intercalator molybdenum disulfide interlayer be rapidly decomposed into gas and by two Molybdenum sulfide particle orientation is scraped, and achievees the purpose that molybdenum disulfide crushes.

The purpose of the present invention can be realized by following technique measures:

The step of preparation method of nano molybdenum disulfide of the invention, is as follows:

A, it configures intercalant solution: weighing intercalator and deionized water is added, configured in mass ratio for 1:0.8-10；

B, molybdenum disulfide is fitted into three mouthfuls of closed containers to (described three mouthfuls of closed containers, one mouth is drain, a mouth is slotting Layer agent solution suction inlet, a mouth are vacuum orifice), by a mouth in three mouthfuls of closed containers by container vacuum-pumping, vacuum Degree control is within the scope of 1.3-60Kpa；The intercalant solution that step a is prepared passes through another mouthful of sucking container of closed container Interior, soakage, which all floods molybdenum disulfide solid with intercalant solution, to be advisable, and opens closed container drain and releases vacuum, extensive Multiple normal pressure, controls immersion 10-24 hours of 20-80 DEG C of temperature；

C, the immersion slurries of step b are filtered, then wash obtained solid molybdenum disulfide after filtering using deionized water, It is dried in vacuo under conditions of 40-60 DEG C of drying temperature later, drying time 2-12 hour；

D, the dried molybdenum disulfide containing intercalator is put into micro-wave oven, regulation power 100-180KW, hold time 5- 60 minutes, nano molybdenum disulfide powder can be obtained using wet classification technology later.

Heretofore described intercalator is derived from any one of ammonium nitrate, sodium nitrate, potassium nitrate or ammonium perchlorate.

It the principle of the present invention and has the beneficial effect that:

1, intercalator is easily rapidly decomposed into gas expansion in a heated state and explodes and generate shock wave, natural molybdenum disulfide Belong to layer structure, combined between layers by weak interaction force, there is certain gap between layers, pass through intercalator The molybdenum disulfide that solution impregnates can make intercalator enter the molecule interlayer of molybdenum disulfide, after vacuum drying, molybdenum disulfide surface and The moisture of interlayer is volatilized, and intercalator is then trapped in molybdenum disulfide interlayer, and heat can swash intercalator in the dry state Strong decomposition rapid gas generating is expanded and is exploded, and molybdenum disulfide particles are burst apart to reach by the energy of this gas rapid expanding The purpose for keeping molybdenum disulfide particles broken.It should be noted that this explosion is not traditional explosion, because of curing Intercalator between molybdenum layer be it is micro, so-called detonation is the detonation in microcosmic meaning, and the invisible explosion phenomenon of macroscopic view will not produce Raw insecurity factor.

2, the nano molybdenum disulfide even particle size distribution prepared using method of the invention, nanoscale product high income can Reach 40% or more, added value of product can be improved.

It 3, will not be because of physical friction band present method avoids the high energy consumption for using supersonic pneumatic milling to crush Enter impurity.

4, the intercalator raw material that method of the invention uses is easy to get, and price is low, and manufacturing cost is low.

Specific embodiment

The present invention is further described below with reference to embodiment:

Embodiment 1:

Ammonium nitrate 20g is weighed, deionized water 80ml is added, is made into intercalant solution；Molybdenum disulfide (D50=10 μm) 20g is packed into In tri- mouthfuls of reaction flasks of 250ml, by a mouth in three mouthfuls of reaction flasks by container vacuum-pumping, vacuum degree control will match in 20Kpa The intercalant solution of system is sucked in three mouthfuls of reaction flasks by another mouth of three mouthfuls of reaction flasks, and soakage is with intercalant solution whole Flooding molybdenum disulfide solid is advisable, and opens closed container drain and vacuum is released to extensive, multiple normal pressure, control temperature 60 C immersion 10 Hour；Slurries filtering will be impregnated, obtained solid molybdenum disulfide is washed one time with deionized water, vacuum drying, and 60 DEG C of drying temperature, Drying time 6 hours；The dried molybdenum disulfide containing intercalator is put into micro-wave oven, regulation power 136KW holds time It 15 minutes, takes out, nanoscale molybdenum disulfide powder 8g is obtained using wet classification technology, granularity D50 is 90nm.The wet process point Well known method can be used to realize in grade method.

Embodiment 2:

Potassium nitrate 50g is weighed, deionized water 150ml is added, is made into intercalant solution；By common molybdenum disulfide (D50=21 μm) 30g is fitted into tri- mouthfuls of reaction flasks of 250ml, and by a mouth in three mouthfuls of reaction flasks by container vacuum-pumping, vacuum degree control exists 6.5Kpa, by the intercalant solution of preparation by the way that in three mouthfuls of reaction flasks of another mouthful of sucking of three mouthfuls of reaction flasks, soakage is with intercalation Agent solution, which all floods molybdenum disulfide solid, to be advisable, and opens closed container drain and releases vacuum, restore normal pressure, controls temperature 50 DEG C are impregnated 8 hours；Slurries filtering will be impregnated, obtained solid molybdenum disulfide is washed three times with deionized water, is dried in vacuo, dry Temperature 50 C, drying time 6 hours.The dried molybdenum disulfide containing intercalator is put into micro-wave oven, regulation power 160KW holds time 10 minutes, takes out, obtaining nanoscale molybdenum disulfide powder 15g, granularity D50 using wet classification technology is 110nm。

Embodiment 3:

Ammonium perchlorate 20g is weighed, value range of the deionized water 150ml(as exceeding 1:0.8-10 is added), it is molten to be made into intercalator Liquid；Common molybdenum disulfide (D50=6 μm) 10g is fitted into tri- mouthfuls of reaction flasks of 250ml, is vacuumized, vacuum degree control exists 1.39Kpa, by the intercalant solution of preparation by the way that in three mouthfuls of reaction flasks of another mouthful of sucking of three mouthfuls of reaction flasks, soakage is with intercalation Agent solution, which all floods molybdenum disulfide solid, to be advisable, and opens closed container drain and releases vacuum, restore normal pressure, controls temperature 40 DEG C are impregnated 6 hours；Slurries filtering will be impregnated, obtained solid molybdenum disulfide is washed one time with deionized water, is dried in vacuo, dry Temperature 60 C, drying time 8 hours.The dried molybdenum disulfide containing intercalator is put into micro-wave oven, regulation power 120KW holds time 30 minutes, takes out, obtaining nanoscale molybdenum disulfide powder 3g, granularity D50 using wet classification technology is 56nm。

Claims (2)

1. a kind of preparation method of nano molybdenum disulfide, it is characterised in that: the method comprises the following steps:

A, it configures intercalant solution: weighing intercalator and deionized water is added, configured in mass ratio for 1:0.8-10；

B, molybdenum disulfide is fitted into three mouthfuls of closed containers, by a mouth in three mouthfuls of closed containers by container vacuum-pumping, very Reciprocal of duty cycle controls within the scope of 1.3-60Kpa；The intercalant solution that step a is prepared is held by another mouthful of sucking of closed container In device, soakage, which all floods molybdenum disulfide solid with intercalant solution, to be advisable, and opens closed container drain and releases vacuum, Restore normal pressure, controls immersion 10-24 hours of 20-80 DEG C of temperature；

C, the immersion slurries of step b are filtered, then wash obtained solid molybdenum disulfide after filtering using deionized water, It is dried in vacuo under conditions of 40-60 DEG C of drying temperature later, drying time 2-12 hour；

D, the dried molybdenum disulfide containing intercalator is put into micro-wave oven, regulation power 100-180KW, hold time 5- 60 minutes, nano molybdenum disulfide powder can be obtained using wet classification technology later.

2. the preparation method of nano molybdenum disulfide according to claim 1, it is characterised in that: the intercalator is derived from nitre Any one of sour ammonium, sodium nitrate, potassium nitrate or ammonium perchlorate.