CN108394936A - The preparation method of molybdenum disulfide-Palygorskite Nanometer rod composite material - Google Patents
The preparation method of molybdenum disulfide-Palygorskite Nanometer rod composite material Download PDFInfo
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- CN108394936A CN108394936A CN201810358799.XA CN201810358799A CN108394936A CN 108394936 A CN108394936 A CN 108394936A CN 201810358799 A CN201810358799 A CN 201810358799A CN 108394936 A CN108394936 A CN 108394936A
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- C01G39/00—Compounds of molybdenum
- C01G39/06—Sulfides
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Abstract
The preparation method of molybdenum disulfide Palygorskite Nanometer rod composite material of the present invention, is related to composite material, prepares tool molybdenum disulfide Palygorskite Nanometer rod composite material using microwave-hydrothermal method, step is：Prepare the reactant feed mixed liquor of molybdate, sulfide and Palygorskite Nanometer stick；By the reactant feed mixed liquor pour into ptfe autoclave be placed in microwave hydrothermal equipment complete reactant microwave-hydrothermal method it is effectively compound；Molybdenum disulfide Palygorskite Nanometer rod composite material is made in the washed drying of microwave-hydrothermal method products therefrom.The prior art prepared the present invention overcomes molybdenum disulfide composite material molybdenum disulfide composite material in drying or annealing process is easy to reassemble or stack and preparation process is complicated, reaction time is long, high energy consumption and defect of high cost.
Description
Technical field
Technical scheme of the present invention is related to composite material, specifically molybdenum disulfide-Palygorskite Nanometer rod composite material
Preparation method.
Background technology
Molybdenum disulfide is a kind of typical stratiform transient metal sulfide, every two layers of sulphur atom layer sandwich, one layer of molybdenum original
Sublayer forms typical sandwich structure, is covalent bond between molybdenum atom and sulphur atom, between adjacent two molecular layer by comparing
Weak Van der Waals force is connected, and effect is compared with strong, interlaminar action is relatively weak in layer.Due to this special layer structure so that
Molybdenum disulfide has good catalysis, lubrication and the performances such as photoelectricity, be widely used in lithium ion cell electrode and photocatalysis,
Solid lubrication, sensor, field-effect transistor technical field.
Molybdenum disulfide is since the unsaturation of its structural edge has higher reactivity, in addition, molybdenum disulfide is narrow
Gap semiconductor has preferable assimilation effect to visible light, in terms of having been applied in photocatalysis.Following documents reports curing
Application of the molybdenum in photocatalysis field：Document MoS2-GO nanocomposites synthesized via a
hydrothermal hydrogel method for solar light photocatalytic degradation of
methylene blue(Y Ding,Y Zhou,W Nie,et al.MoS2-GO nanocomposites synthesized
via a hydrothermal hydrogel method for solar light photocatalytic degradation
of methylene blue[J].Applied Surface Science,2015,357:1606-1612.) describe using one
One-step hydrothermal prepares MoS2- GO hydrogel composite materials；CN107233900A discloses a kind of molybdenum disulfide composite Nano golden light
Catalyst and preparation method thereof；CN106902847A disclose a kind of molybdenum disulfide/barium titanate ultrasound visible light catalyst and its
Preparation and application.In photocatalysis field application, the molybdenum disulfide nano sheet of prior art preparation is easily reunited, and makes exposure
Active site is reduced, and influences giving full play to for photocatalysis performance, the above-mentioned existing skill for preparing molybdenum disulfide composite photocatalyst material
Art is long there is also the period, manufacturing cost is higher, preparation process is complicated and the higher many defects of energy consumption.
Cathode of the molybdenum disulfide as lithium ion battery, is easy to the insertion of lithium ion since interlamellar spacing is larger, can make to fill
Discharge capacity is effectively increased, but leads to lithium ion battery since particle crushes during the lithiumation-repeated takes off lithium
The cyclical stability of charge and discharge is poor.To solve the above-mentioned problems, the negative material for being used as lithium ion battery in the prior art is main
Using the composite material of two kinds of molybdenum disulfide, i.e. molybdenum disulfide-graphene composite material and molybdenum disulfide-carbon composite.Text
Offer Facile synthesis and electrochemical properties of two dimensional layered
MoS2/graphene composite for reversible lithium storage(X Zhou,Z Wang,W Chen,
et al.Facile synthesis and electrochemical properties of two dimensional
layered MoS2/graphene composite for reversible lithium storage[J].Journal of
Power Sources,2014,251(2):It 264-268.) describes and molybdenum disulfide/graphene composite wood is prepared using hydro-thermal method
Material；CN107394184A discloses a kind of molybdenum disulfide/graphene nano belt composite with loose three-dimensional winding arrangement
And its preparation method and application；CN104319102A discloses that a kind of to prepare the three-dimensional flower-shaped graphene/molybdenum disulfide of load compound
Method of the threadiness of material to electrode；Above-mentioned molybdenum disulfide-graphene composite material defect of the existing technology for preparing is：
Such composite material is easy to reassemble or stack in drying or annealing process, this greatly reduces specific surface area, limits
The transport of electronics and ion also needs to high annealing in some preparation methods, and manufacturing cycle is longer, cost is higher.
CN107256949A discloses the preparation method of platelike molybdenumdisulfide/carbon composite；CN104966817A discloses curing
The three-dimensional porous network composite material and preparation method of molybdenum and carbon；CN107275600A disclose the molybdenum disulfide of hollow sphere/
The preparation method of carbon composite；CN106423218A discloses a kind of synthetic method of molybdenum disulfide/carbon nano-composite material；
CN104934602A discloses a kind of molybdenum disulfide/carbon composite and preparation method thereof；CN106410136A discloses one kind
Layer structure molybdenum disulfide/carbon composite and the preparation method and application thereof；It is above-mentioned that prepare molybdenum disulfide-carbon composite existing
Technology has a defect that：It carries out compound being the carbon material synthesized by carbon source with molybdenum disulfide, wherein use sol-gel
The entire experimental period of method is longer；Need to introduce template using hydro-thermal method, and template also needs to handle or remove again；Using change
That learns vapour deposition process needs progress high temperature vapor deposition, and combined coefficient is relatively low and easy tos produce by-product, influences product quality.
The method of prior art preparation molybdenum disulfide composite material mainly has chemical vapour deposition technique, high temperature solid-state method, is total to
The precipitation method, sol-gel method and hydro-thermal method.Chemical vapour deposition technique requires experiment condition high, controllability and poor repeatability.It is high
Warm solid phase method prepares that larger product granularity, high energy consumption, efficiency are low, are easy to be mixed into impurity.Coprecipitation reacts complicated in the liquid phase,
Control difficulty is big, may will produce reunion when precipitating reagent is added or composition is not uniform enough.Raw material used in sol-gel method is normal
It is related to organic matter and expensive, it is longer the time required to entire sol-gel process.Existing hydro-thermal method is long there are reaction time,
The defect of high energy consumption.
Invention content
The technical problem to be solved by the present invention is to：The preparation side of molybdenum disulfide-Palygorskite Nanometer rod composite material is provided
Method is to prepare molybdenum disulfide-palygorskite using microwave-hydrothermal method using molybdate, sulfide and Palygorskite Nanometer stick as raw material
Nanometer rod composite material, overcome molybdenum disulfide composite material preparation the prior art in drying or annealing process molybdenum disulfide
Composite material is easy to reassemble or stack and preparation process is complicated, reaction time is long, high energy consumption and defect of high cost.
Technical solution is used by the present invention solves the technical problem：Molybdenum disulfide-Palygorskite Nanometer rod composite material
Preparation method, be as follows：
The first step, the preparation of reactant feed mixed liquor：
The molybdate, 10~150mmol sulfide and 0.1~2.0g Palygorskite Nanometer sticks of 1~20mmol are weighed respectively,
First molybdate is dissolved in 35~175mL deionized waters, it is to be mixed to be completely dissolved to molybdate then the sulfide weighed is molten
In above-mentioned molybdate solution, 20~50min of magnetic agitation at room temperature will be alleged after liquid to be mixed is in homogeneous transparent state
The Palygorskite Nanometer stick taken is added, at room temperature 30~60min of magnetic agitation, then 10~30min of ultrasound, and it is former to complete reactant
Expect the preparation of mixed liquor；
The microwave-hydrothermal method of second step, reactant is effectively compound：
The reactant feed mixed liquor that the above-mentioned first step is prepared is poured into the polytetrafluoroethylene (PTFE) that volume is 50~250mL
In reaction kettle, compactedness is 50%~70%, which is placed in microwave hydrothermal equipment, and setting temperature is
170~230 DEG C, pressure is that 2~4MPa is cooled to room temperature, the microwave-hydrothermal method for completing reactant is effectively multiple after keeping the temperature 1~5h
It closes；
Third walks, and prepares molybdenum disulfide-Palygorskite Nanometer rod composite material：
The microwave-hydrothermal method effectively compound obtained product that above-mentioned second step is completed to reactant, 4 are carried out with deionized water
~6 washings, dry 12 under the conditions of temperature is 60~80 DEG C~for 24 hours, obtain molybdenum disulfide-Palygorskite Nanometer stick composite wood
Material.
The preparation method of above-mentioned molybdenum disulfide-Palygorskite Nanometer rod composite material, the molybdate are ammonium molybdate, magnesium molybdate
Or alkali metal molybdate.
The preparation method of above-mentioned molybdenum disulfide-Palygorskite Nanometer rod composite material, the sulfide are thioacetamide, sulphur
Urea or L-cysteine.
The preparation method of above-mentioned molybdenum disulfide-Palygorskite Nanometer rod composite material, the microwave hydrothermal equipment are multipurpose
Microwave chemosynthesis instrument, microwave hydrothermal reaction or microwave hydrothermal parallel projects instrument.
The preparation method of above-mentioned molybdenum disulfide-Palygorskite Nanometer rod composite material, the compactedness are that filler accounts for poly- four
The percent by volume of vinyl fluoride reaction kettle.
The preparation method of above-mentioned molybdenum disulfide-Palygorskite Nanometer rod composite material, the raw material Palygorskite Nanometer stick be by
Prepared by method disclosed in ZL201610520132.6, other raw materials are commercially available, and involved equipment is ability
Well known to domain, involved process operation is that those skilled in the art will appreciate that.
The beneficial effects of the invention are as follows：Compared with prior art, substantive distinguishing features outstanding possessed by the present invention are as follows：
(1) palygorskite is the porous clay mineral of zeopan containing Shuifu County of a kind of layer of chain structure, belong to orthorhombic system or
Monoclinic system, crystal-chemical formula Mg2Al2Si8O20(OH)2(OH2)4·4H2O.In palygorskite Mg, Al, O octahedral layer and
Alternately superposition forms the structure with layer chain and multi-pore channel to Si, O tetrahedral layer, just because it has this special structure so that
There are a large amount of zeolite aquaporins and holes inside palygorskite, have big specific surface area, have absorption, rheology, catalysis, friction and
The performance of dispersion can be used for adsorbing, be catalyzed and lubrication technical field.
Molybdenum disulfide is carried on Palygorskite Nanometer stick by the present invention, the two can under certain condition shown excellent
Synergistic effect.Reason is：Molybdenum disulfide nano sheet is easily reunited, and so that exposed active site is reduced, is influenced photocatalysis
Etc. performances give full play to.And large specific surface area, the good dispersion of Palygorskite Nanometer stick, Palygorskite Nanometer stick is introduced as function
Carrier regulation and control molybdenum disulfide nano sheet structure can effectively reduce curing while improving molybdenum disulfide nano sheet pattern
The reunion of molybdenum nanometer sheet increases the active site quantity of material.Therefore, molybdenum disulfide-Palygorskite Nanometer stick that the present invention is built
Composite material not only has important theory significance, is also with a wide range of applications.
(2) the method for the present invention utilizes the property of Palygorskite Nanometer stick, the serious flower-shaped molybdenum disulfide that can will reunite micro-
It is evenly dispersed nanometer sheet that spherical structure, which improves, and the nanometer sheet is regularly grown on Palygorskite Nanometer stick, to
A kind of novel molybdenum disulfide-Palygorskite Nanometer rod composite material is arrived.
(3) compared with prior art, the present invention has following substantive distinguishing characteristics：
1) CN107233900A discloses a kind of molybdenum disulfide composite nano-gold photochemical catalyst and preparation method thereof, this is compound
Material is to first pass through chemical synthesis to prepare spherical molybdenum disulfide nano particle, then be prepared using sol-gel method.It prepares
Complex process, complex steps, the period is longer, and also needs to calcine in nitrogen atmosphere high temperature, and energy consumption is higher.The present invention utilizes day
Right mineral are effectively compound by microwave-hydrothermal method progress with molybdenum disulfide, are effectively improved while with the shorter reaction time
The pattern of molybdenum disulfide；Compared with gold chloride, palygorskite also has many advantages, such as cheap, resourceful as natural minerals.
2) CN106902847A discloses a kind of molybdenum disulfide/barium titanate ultrasound visible light catalyst and its prepares and answer
With the preparation of the molybdenum disulfide/barium titanate composite material uses hydro-thermal method, manufacturing cycle longer.The present invention utilizes natural minerals
It is effectively compound by microwave-hydrothermal method progress with molybdenum disulfide, two sulphur are effectively improved while with more short reaction time
Change the pattern of molybdenum, and compare barium titanate, the palygorskite that the present invention uses also has the advantages that cheap and resourceful.
3) it is multiple to disclose a kind of molybdenum disulfide/graphene nanobelt with loose three-dimensional winding arrangement by CN107394184A
Condensation material and its preparation method and application, the preparation of the composite material is other than using hydro-thermal method, it is also necessary to high annealing, energy consumption
It is higher.The present invention be carried out by microwave-hydrothermal method using natural minerals and molybdenum disulfide it is effectively compound, with shorter anti-
The pattern of molybdenum disulfide is effectively improved while between seasonable；Compared with graphene, palygorskite also has price as natural minerals
The advantages that cheap, resourceful.
4) CN104319102A discloses a kind of fiber for preparing and loading three-dimensional flower-shaped graphene/molybdenum disulfide composite material
Shape is to the method for electrode, and using hydro-thermal method, manufacturing cycle is longer for the preparation of the molybdenum disulfide/graphene composite material.The present invention
It is effectively compound by microwave-hydrothermal method progress with molybdenum disulfide using natural minerals, it is effective while with more short reaction time
Ground improves the pattern of molybdenum disulfide；Compared to graphene oxide, the palygorskite that the present invention uses also has cheap and money
The abundant advantage in source.
5) CN107256949A discloses the preparation method of platelike molybdenumdisulfide/carbon composite, in the preparation method with
Molybdenum disulfide carries out compound being the carbon material synthesized by carbon source, needs high-temperature calcination in an inert atmosphere, energy consumption higher.This
Outside, longer entire experimental period using sol-gel method.The present invention passes through microwave-hydrothermal method using natural minerals and molybdenum disulfide
Progress is effectively compound, and the pattern of molybdenum disulfide is effectively improved while with the shorter reaction time；Compared with carbon material, slope
Thread masonry also has many advantages, such as cheap, resourceful for natural minerals.
6) CN104966817A discloses the three-dimensional porous network composite material and preparation method of molybdenum disulfide and carbon, the system
It carries out with molybdenum disulfide compound being carbon material in Preparation Method, needs to calcine in argon gas atmosphere high temperature, energy consumption is higher.In addition,
Using chemical vapour deposition technique, require height, combined coefficient relatively low experiment condition.The present invention utilizes natural minerals and molybdenum disulfide
It is effectively compound by microwave-hydrothermal method progress, the pattern of molybdenum disulfide is effectively improved while with the shorter reaction time；
Compared with carbon material, palygorskite also has many advantages, such as cheap, resourceful as natural minerals.
7) CN107275600A discloses the preparation method of molybdenum disulfide/carbon composite of hollow sphere, the preparation side
It carries out with molybdenum disulfide compound being carbon material in method, complex process needs to introduce template, and templated silicas is wasted
Fall, uses hydro-thermal method longer experimental period in addition.The present invention is carried out with molybdenum disulfide by microwave-hydrothermal method using natural minerals
It is effectively compound, the pattern of molybdenum disulfide is effectively improved while with the shorter reaction time；Compared with carbon material, palygorskite
Also have many advantages, such as natural minerals cheap, resourceful.
8) CN106423218A discloses a kind of synthetic method of molybdenum disulfide/carbon nano-composite material, the preparation method
In carry out compound being carbon material with molybdenum disulfide, need high-temperature calcination under an inert atmosphere, energy consumption is higher, is by metal in addition
It after molybdenum ion is complexed with humic acid essence potassium, then calcines with sodium sulphate mixed grinding, may mix uneven, cause product uneven
It is even, it is second-rate.The present invention is effectively compound by microwave-hydrothermal method progress with molybdenum disulfide using natural minerals, with more
The pattern of molybdenum disulfide is effectively improved while the short reaction time；Compared with carbon material, palygorskite also has as natural minerals
Have the advantages that cheap, resourceful.
9) CN104934602A discloses a kind of molybdenum disulfide/carbon composite and preparation method thereof, in the preparation method
It carries out compound being carbon material with molybdenum disulfide, complex process, complex steps, cost are higher, and need by high-temperature calcination, energy
Consumption is higher.The present invention is effectively compound by microwave-hydrothermal method progress with molybdenum disulfide using natural minerals, with shorter
The pattern of molybdenum disulfide is effectively improved while reaction time；Compared with carbon material, palygorskite also has valence as natural minerals
The advantages that lattice are cheap, resourceful.
10) CN106410136A discloses a kind of layer structure molybdenum disulfide/carbon composite and preparation method thereof and answers
With carrying out with molybdenum disulfide compound being carbon material in the preparation method, complex process needs to carry out high temperature vapor deposition, energy
Consumption is higher, and has hydrogen sulfide gas and generate and enter environment, and there is corrosivity also to easy to produce by-product.The present invention is to utilize day
Right mineral are effectively compound by microwave-hydrothermal method progress with molybdenum disulfide, are effectively improved while with the shorter reaction time
The pattern of molybdenum disulfide；Compared with carbon material, palygorskite also has many advantages, such as cheap, resourceful as natural minerals.
(4) in the prior art, there is not yet related prepare molybdenum disulfide-Palygorskite Nanometer stick composite wood using microwave-hydrothermal method
The document report of material.
Compared with prior art, the present invention has marked improvement as follows：
(1) the method for the present invention is using molybdate, sulfide and Palygorskite Nanometer stick as raw material, using microwave hydrothermal legal system
Standby molybdenum disulfide-Palygorskite Nanometer rod composite material overcomes gained molybdenum disulfide in the prior art and its composite material dry
It is easy to reassemble or stack in dry or annealing process and preparation process is complicated, the period is long, high energy consumption and of high cost lacks
It falls into.
(2) palygorskite has many advantages, such as cheap, resourceful as natural minerals, adds to natural resources natural minerals
To utilize, its application range is widened and has saved cost.
(3) the method for the present invention can be effectively improved the pattern of molybdenum disulfide, and product pattern is good and uniform, and prepares work
Skill has good repeatability.
(4) the method for the present invention uses microwave-hydrothermal method, reaction to be done directly in the liquid phase, and reaction dissolvent only has deionization
Water, preparation process green, environmental protection, economical while easy to operate, reaction time is short.
Description of the drawings
Fig. 1 is the scanning electron microscopic picture of molybdenum disulfide-Palygorskite Nanometer rod composite material prepared by the method for the present invention.
Specific implementation mode
Fig. 1 is the scanning electron microscopic picture of molybdenum disulfide-Palygorskite Nanometer rod composite material prepared by the method for the present invention.It is existing
It is the shapes such as flower-like microsphere that molybdenum disulfide nano sheet prepared by technical method, which is easy to reunite, dispersed poor.The figure shows this hair
Bright introducing Palygorskite Nanometer stick as function carrier, make molybdenum disulfide dimensional homogeneity and dispersibility be improved significantly, and
The nanometer sheet is regularly grown on Palygorskite Nanometer stick, to obtain a kind of novel molybdenum disulfide-Palygorskite Nanometer
Rod composite material.
Embodiment 1
The first step, the preparation of reactant feed mixed liquor：
The ammonium molybdate, 10mmol thioacetamides and 0.1g Palygorskite Nanometer sticks for weighing 1mmol respectively, first by ammonium molybdate
It is dissolved in 35mL deionized waters, it is to be mixed to be completely dissolved to ammonium molybdate, then the thioacetamide weighed is dissolved in above-mentioned molybdic acid
In ammonium salt solution, magnetic agitation 20min at room temperature, after liquid to be mixed is in homogeneous transparent state, the Palygorskite Nanometer that will be weighed
Stick is added, at room temperature magnetic agitation 30min, then ultrasound 10min, completes the preparation of reactant feed mixed liquor；
The microwave-hydrothermal method of second step, reactant is effectively compound：
The reactant feed mixed liquor that the above-mentioned first step is prepared is poured into the polytetrafluoroethyl-ne alkene reaction that volume is 50mL
In kettle, which is placed in multipurpose microwave chemosynthesis instrument by compactedness 50%, and setting temperature is
It 170 DEG C, pressure 2MPa, after keeping the temperature 1h, is cooled to room temperature, the microwave-hydrothermal method for completing reactant is effectively compound；
Third walks, and prepares molybdenum disulfide-Palygorskite Nanometer rod composite material：
The microwave-hydrothermal method effectively compound obtained product that above-mentioned second step is completed to reactant, 4 are carried out with deionized water
Secondary washing, dry 12h, obtains molybdenum disulfide-Palygorskite Nanometer rod composite material under the conditions of temperature is 60 DEG C.
Embodiment 2
The first step, the preparation of reactant feed mixed liquor：
Magnesium molybdate, is first dissolved in by the magnesium molybdate, 80mmol thiocarbamides and 1.0g Palygorskite Nanometer sticks for weighing 10mmol respectively
It is to be mixed to be completely dissolved to magnesium molybdate in 100mL deionized waters, then the thiocarbamide weighed is dissolved in above-mentioned molybdic acid magnesium solution,
The Palygorskite Nanometer stick weighed is added in after homogeneous transparent state for magnetic agitation 35min at room temperature, liquid to be mixed,
Magnetic agitation 45min at room temperature, then ultrasound 20min, completes the preparation of reactant feed mixed liquor；
The microwave-hydrothermal method of second step, reactant is effectively compound：
The reactant feed mixed liquor that the above-mentioned first step is prepared is poured into the polytetrafluoroethyl-ne alkene reaction that volume is 150mL
In kettle, which is placed in microwave hydrothermal reaction by compactedness 60%, and setting temperature is 200 DEG C, pressure
Power is 3MPa, after keeping the temperature 3h, is cooled to room temperature, the microwave-hydrothermal method for completing reactant is effectively compound；
Third walks, and prepares molybdenum disulfide-Palygorskite Nanometer rod composite material：
The microwave-hydrothermal method effectively compound obtained product that above-mentioned second step is completed to reactant, 5 are carried out with deionized water
Secondary washing, dry 18h, obtains molybdenum disulfide-Palygorskite Nanometer rod composite material under the conditions of temperature is 70 DEG C.
Embodiment 3
The first step, the preparation of reactant feed mixed liquor：
The alkali metal molybdate, 150mmolL- cysteines and 2.0g Palygorskite Nanometer sticks of 20mmol are weighed respectively, first
Alkali metal molybdate is dissolved in 175mL deionized waters, it is to be mixed to be completely dissolved to alkali metal molybdate, then the L- that will be weighed
Cysteine is dissolved in above-mentioned alkali metal molybdate solution, at room temperature magnetic agitation 50min, and liquid to be mixed is in homogeneous transparent shape
After state, the Palygorskite Nanometer stick weighed is added, at room temperature magnetic agitation 60min, then ultrasound 30min, completes reaction
The preparation of raw material mixed liquor；
The microwave-hydrothermal method of second step, reactant is effectively compound：
The reactant feed mixed liquor that the above-mentioned first step is prepared is poured into the polytetrafluoroethyl-ne alkene reaction that volume is 250mL
In kettle, which is placed in microwave hydrothermal parallel projects instrument by compactedness 70%, and setting temperature is 230
DEG C, pressure 4MPa is cooled to room temperature, the microwave-hydrothermal method for completing reactant is effectively compound after keeping the temperature 5h；
Third walks, and prepares molybdenum disulfide-Palygorskite Nanometer rod composite material：
The microwave-hydrothermal method effectively compound obtained product that above-mentioned second step is completed to reactant, 6 are carried out with deionized water
Secondary washing is dried for 24 hours under the conditions of temperature is 80 DEG C, obtains molybdenum disulfide-Palygorskite Nanometer rod composite material.
In above-described embodiment, the compactedness is the percent by volume that filler accounts for ptfe autoclave；The original
Expect that palygorskite nanometer rods are according to prepared by method disclosed in ZL201610520132.6, other raw materials are commercially available,
What involved equipment was known in the art, involved process operation is that those skilled in the art will appreciate that.
Claims (4)
1. the preparation method of molybdenum disulfide-Palygorskite Nanometer rod composite material, it is characterised in that be as follows：
The first step, the preparation of reactant feed mixed liquor：
The molybdate, 10~150mmol sulfide and 0.1~2.0g Palygorskite Nanometer sticks of 1~20mmol are weighed respectively, first will
Molybdate is dissolved in 35~175mL deionized waters, to be mixed to be completely dissolved to molybdate, then the sulfide weighed is dissolved in
State in molybdate solution, at room temperature 20~50min of magnetic agitation, liquid to be mixed be in homogeneous transparent state after, by what is weighed
Palygorskite Nanometer stick is added, at room temperature 30~60min of magnetic agitation, then 10~30min of ultrasound, and it is mixed to complete reactant feed
Close the preparation of liquid；
The microwave-hydrothermal method of second step, reactant is effectively compound：
The reactant feed mixed liquor that the above-mentioned first step is prepared is poured into the polytetrafluoroethyl-ne alkene reaction that volume is 50~250mL
In kettle, compactedness be 50%~70%, which is placed in microwave hydrothermal equipment, setting temperature be 170~
230 DEG C, pressure is that 2~4MPa is cooled to room temperature, the microwave-hydrothermal method for completing reactant is effectively compound after keeping the temperature 1~5h；
Third walks, and prepares molybdenum disulfide-Palygorskite Nanometer rod composite material：
The microwave-hydrothermal method effectively compound obtained product that above-mentioned second step is completed to reactant, is carried out 4~6 times with deionized water
Washing, dry 12 under the conditions of temperature is 60~80 DEG C~for 24 hours, obtain molybdenum disulfide-Palygorskite Nanometer rod composite material.
2. the preparation method of molybdenum disulfide-Palygorskite Nanometer rod composite material according to claim 1, it is characterised in that：Institute
It is ammonium molybdate, magnesium molybdate or alkali metal molybdate to state molybdate.
3. the preparation method of molybdenum disulfide-Palygorskite Nanometer rod composite material according to claim 1, it is characterised in that：Institute
It is thioacetamide, thiocarbamide or L-cysteine to state sulfide.
4. the preparation method of molybdenum disulfide-Palygorskite Nanometer rod composite material according to claim 1, it is characterised in that：Institute
It is multipurpose microwave chemosynthesis instrument, microwave hydrothermal reaction or microwave hydrothermal parallel projects instrument to state microwave hydrothermal equipment.
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| CN113149078A (en) * | 2021-04-07 | 2021-07-23 | 安徽文达信息工程学院 | Preparation method of attapulgite-based molybdenum disulfide composite microwave absorbent |
| CN114259981A (en) * | 2021-12-23 | 2022-04-01 | 武汉大学(肇庆)资源与环境技术研究院 | Clay mineral loaded molybdenum disulfide composite material and preparation method and application thereof |
| CN114259981B (en) * | 2021-12-23 | 2024-05-24 | 武汉大学(肇庆)资源与环境技术研究院 | Clay mineral loaded molybdenum disulfide composite material and preparation method and application thereof |
| CN115418259A (en) * | 2022-09-20 | 2022-12-02 | 西南交通大学 | Lubricating grease thickening agent and preparation method thereof, and lubricating grease and preparation method thereof |
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