CN109734131A - A kind of ultra-high throughput stripping means of transient metal sulfide - Google Patents
A kind of ultra-high throughput stripping means of transient metal sulfide Download PDFInfo
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- CN109734131A CN109734131A CN201910058060.1A CN201910058060A CN109734131A CN 109734131 A CN109734131 A CN 109734131A CN 201910058060 A CN201910058060 A CN 201910058060A CN 109734131 A CN109734131 A CN 109734131A
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- metal sulfide
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Abstract
The present invention relates to a kind of ultra-high throughput stripping means of transient metal sulfide.Specifically: (1) aqueous solution or organic solvent solution of transient metal sulfide powder and auxiliary agent are mixed, forms viscous paste；(2) the corresponding solvent of the viscous paste of formation is diluted, transient metal sulfide dispersion liquid is obtained after stirring；(3) slurry in (1) or the dispersion liquid in (2) are dried, obtain addition agent modified transient metal sulfide powder；(4) by product obtained in (3) under inert gas or vacuum condition high-temperature process, obtain pure transient metal sulfide powder.It removes concentration greater than 200 mg/mls to the present invention, reaches as high as 600 mg/mls, is 10-100 times of conventional stripping methods.Safe preparation process of the present invention is controllable, flux is high, is easier to industrial amplification, and no pollution to the environment.The method of the present invention is at low cost, efficiently solves the critical issue of transient metal sulfide material prepare with scale, to realize that the practical application of transient metal sulfide provided possibility.
Description
Technical field
The invention belongs to field of material technology, are related to a kind of ultra-high throughput stripping means of transient metal sulfide, specifically
For by transient metal sulfide powder in the aqueous solution of auxiliary agent or organic solution ball milling or be sanded a period of time after, formed it is sticky
Slurry；Slurry with water will be formed by or the dilution of corresponding solvent, stirring obtained transient metal sulfide dispersion liquid after 30 minutes；
Gained slurry or dispersion liquid are dried, addition agent modified transient metal sulfide powder is obtained；By gained powder in inertia
High-temperature process under gas or vacuum condition obtains pure transient metal sulfide powder.
Background technique
Transient metal sulfide has caused the extensive concern of academia and industrial circle with its excellent comprehensive performance.It crosses
It crosses the unique structural advantage of metal sulfide and imparts the properties such as its electricity abundant, optics, mechanics, convert and deposit in energy
The fields such as storage, high-performance composite materials, biology have wide practical use.In order to realize answering on a large scale for transient metal sulfide
With, develop it is a kind of be simple and efficient, low cost, low pollution preparation method seem most important.With the preparation method of graphene
Similar, the preparation method of transient metal sulfide can be divided into measures major class from top to bottom and from bottom to top.Wherein, with transition metal
Ontology is that the liquid phase stripping means of raw material is a kind of method from top to bottom for being considered to have fine industrial prospect.This method is usually
Sulfide powders are dispersed in suitable organic solvent or aqueous surfactant solution, it is strong outer in ultrasound, shearing or ball milling etc.
Under power effect, the removing of transient metal sulfide is realized.However, traditional liquid phase stripping means flux is low, i.e., its remove concentration,
The lot of essential factors such as removing yield, dispersion concentration are unable to satisfy industrialized needs.Currently, the most successful stripping of transient metal sulfide
It is alkali metal intercalation stripping method from method.Although the removing yield of such method is higher, alkali metal to empty gas and water etc. very
Sensitivity, experiment condition is harsh and risk is big, it is difficult to industry amplification.In addition, the removing concentration of current transient metal sulfide
It is lower, usually in 20 mg/mls or so, it is unable to satisfy industrial demand.Thus, develop high-throughput, low cost, letter
Transient metal sulfide preparation method that is single efficient and being easy to industry amplification seems most important.
A kind of ultra-high throughput stripping means for transient metal sulfide that the present invention reports.Compared with conventional stripping methods,
The substantive characteristics of this method is (1), and it removes concentration more than 200 mg/mls, reaches as high as 600 mg/mls；(2)
Being completely exfoliated for transient metal sulfide can be achieved, removing yield is handled close to 100% without further method classification, removing gained
The thickness of transient metal sulfide nanometer sheet in 5 atomic layer level thickness hereinafter, and stripping process will not destroy the crystalline substance of sulfide
Lattice structure；(3) the transient metal sulfide energy stable dispersion obtained after removing, room temperature store over 6 months still without obvious sediment.
The present invention solves the critical issue of transient metal sulfide prepare with scale, is that preparation is removed in the scale of two-dimension nano materials
Technical strategies are provided, its practical application will be pushed significantly.
Summary of the invention
It is an object of the invention to overcome above-mentioned difficulties, a kind of ultra-high throughput removing side of transient metal sulfide is provided
Method.The present invention is using ball milling or the mode of action is sanded, and removing concentration is high, and yield is close to 100% and is able to maintain transient metal sulfide
Complete crystal structure is easy to industrial amplification.Transient metal sulfide prepared by the present invention can be dispersed in water and other organic
In solvent, it can apply to the fields such as energy storage, catalysis, composite material.
The invention proposes a kind of ultra-high throughput stripping means of transient metal sulfide, the specific steps are as follows:
(1) transient metal sulfide powder is added in the aqueous solution containing auxiliary agent, after mixing evenly, passes through ball mill or sand
Mill mechanical effect, forms viscous paste；The described transient metal sulfide removing concentration be removing concentration be greater than 200 milligrams/
Milliliter, reaches as high as 600 mg/mls；Auxiliary dosage is 0.1-2 times of transient metal sulfide powder quality；
(2) the viscous paste water or corresponding organic solvent diluting obtained step (1) stirs 30 minutes and forms stable mistake
Cross metal sulfide dispersion liquid；The transient metal sulfide removing concentration is that removing concentration is greater than 200 mg/mls, most
High reachable 600 mg/mls；
(3) place is dried in the viscous paste that step (1) obtains or the transient metal sulfide dispersion liquid that step (2) obtains
Reason, obtains addition agent modified transient metal sulfide powder；
(4) product for obtaining step (3) high-temperature process under inert gas or vacuum condition, obtains pure transient metal sulfide
Powder.
Present inventor, transient metal sulfide described in step (1) includes molybdenum disulfide or tungsten disulfide, and raw materials size is
50 nanometers -100 microns.
Present inventor, step (1) described auxiliary agent includes any in polyvinylpyrrolidone, polyethylene glycol or polyvinyl alcohol
Kind.
Present inventor, organic solvent described in step (1) includes ethyl alcohol, methanol, n,N dimethylformamide, N- methyl pyrrole
It is any in pyrrolidone or ethylene glycol.
Present inventor, sand mill revolving speed described in step (1) are 150-1600 revs/min, and it is that 0.5-24 is small that the time, which is sanded,
When；Drum's speed of rotation is 150-600 revs/min, and Ball-milling Time is 1-24 hours.
Present inventor, the removing concentration of transient metal sulfide described in step (1) are that removing concentration is greater than 200 milligrams/milli
It rises, reaches as high as 600 mg/mls；Auxiliary dosage is 0.1-2 times of transient metal sulfide material quality.
Present inventor, drying process described in step (3) include spray drying, super close on that carbon dioxide is dry, freezing is dry
Dry, vacuum drying or forced air drying.
Present inventor, inert gas described in step (4) includes nitrogen or argon gas.
In view of the deficienciess of the prior art, the present inventor passes through long-term practice and research, skill of the invention is proposed
Art scheme, the program can realize the high throughput, low cost, large scale preparation of transient metal sulfide, solve Transition Metal Sulfur
The critical issue of compound prepare with scale, for realize transient metal sulfide every field (such as energy storage material, composite material,
Catalysis, super lubrication) in practical application provide a kind of effective way.
The present invention has the advantage that compared with prior art
(1) the ultrahigh concentration removing of the achievable transient metal sulfide of the present invention, removing concentration are greater than 200 mg/mls, highest
It removes concentration and is greater than 600 mg/mls.
(2) present invention is able to achieve being completely exfoliated for transient metal sulfide, and removing yield is not necessarily to further method close to 100%
Classification processing.And stripping process will not destroy the lattice structure of transient metal sulfide
(3) the obtained transient metal sulfide of present invention removing can in various solvents stable dispersion, store under normal temperature condition super
It spends 6 months still to undergo no deterioration, convenient for further application.
(4) the invention is simple and feasible, it can be achieved that transient metal sulfide is completely exfoliated, and is easy to industrial amplification.And this hair
Bright stripping process not can cause environmental pollution, and be a kind of green stripping means.
(5) directly purchase business transition gold sulfide powders are raw material, and raw material sources are extensive, low in cost.
Detailed description of the invention
Fig. 1 is the transmission electron microscope photo of gained molybdenum disulfide.As seen from the figure, obtained molybdenum disulfide nano sheet is removed
For size between tens nanometers to several hundred nanometers, almost transparent appearance illustrates that obtained is few layer structure.
Fig. 2 is the high-resolution-ration transmission electric-lens photo of gained molybdenum disulfide.As seen from the figure, obtained molybdenum disulfide nano sheet
The number of plies is generally within 5 layers.
Fig. 3 is the number of plies distribution map of gained molybdenum disulfide.As seen from the figure, the nanometer sheet number of plies more than 80% 2 to 4 layers it
Between.
Fig. 4 is the transmission electron microscope photo of gained tungsten disulfide.As seen from the figure, obtained tungsten disulfide nano slices are removed
For size between tens nanometers to several hundred nanometers, almost transparent appearance illustrates that obtained is few layer structure.
Fig. 5 is the high-resolution-ration transmission electric-lens photo of gained tungsten disulfide.As seen from the figure, obtained molybdenum disulfide nano sheet
The number of plies is generally within 5 layers.
Fig. 6 is the number of plies distribution map of gained tungsten disulfide.As seen from the figure, the nanometer sheet number of plies more than 80% 2 to 4 layers it
Between.
Specific embodiment
Illustrate technical solution of the present invention below by way of specific example.It should be understood that the one or more that the present invention mentions
Step do not repel before and after the combination step there is also between other method and steps or these specifically mentioned steps also
Other method and steps can be inserted.It should also be understood that these examples are merely to illustrate the present invention rather than limitation is of the invention
Range.Unless otherwise indicated, the number of various method steps is only the purpose of identification various method steps, rather than to limit each method
Arrangement order or limit practical range of the invention, relativeness is altered or modified, in no substantial technological content alteration
Under conditions of, when being also considered as the enforceable scope of the present invention.
Embodiment 1
(1) 10 grams of polyvinylpyrrolidones are dissolved under agitation in 25 ml deionized waters, it until completely dissolved, will be molten
(10 microns of molybdenum disulfide feedstock Particle size, 95%) content, which is higher than, to be added in ball grinder, be added for liquid and 20 grams of molybdenum disulfide powders
After ball milling pearl, ball milling 20 hours, obtains viscous paste under the conditions of 300 revs/min；
(2) after diluting viscous paste obtained in step (1) with 480 ml deionized waters, stirring obtains curing in 30 minutes
Molybdenum dispersion liquid；
(3) by dispersion liquid freeze-drying process obtained in step (2), polyvinyl pyrrolidon modified molybdenum disulphide powder is obtained
Body；
(4) powder obtained by step (3) is annealed 1 hour in 700 DEG C of nitrogen atmosphere, obtains pure molybdenum disulfide powder.It moves back
Heating rate during fire is 10 DEG C/min, and initial temperature is room temperature；After annealing, sample is naturally cold in nitrogen atmosphere
But.
Embodiment 2
(1) 10 grams of polyvinylpyrrolidones are dissolved under agitation in 25 ml deionized waters, it until completely dissolved, will be molten
(5 microns of tungsten disulfide feedstock Particle size, 95%) content, which is higher than, to be added in ball grinder, be added for liquid and 20 grams of tungsten disulfide powders
After ball milling pearl, ball milling 20 hours, obtains viscous paste under the conditions of 600 revs/min；
(2) after diluting viscous paste obtained in step (1) with 480 ml deionized waters, stirring obtains curing in 30 minutes
Tungsten dispersion liquid；
(3) by dispersion liquid freeze-drying process obtained in step (2), polyvinyl pyrrolidon modified curing tungsten powder is obtained
Body；
(4) powder obtained by step (3) is annealed 1 hour in 700 DEG C of nitrogen atmosphere, obtains pure tungsten disulfide powder；It moves back
Heating rate during fire is 10 DEG C/min, and initial temperature is room temperature；After annealing, sample is naturally cold in nitrogen atmosphere
But.
Embodiment 3
(1) 10 grams of polyethylene glycol are dissolved under agitation in 25 ml deionized waters, until completely dissolved, by solution and 20
(100 microns of molybdenum disulfide feedstock Particle size, 95%) content, which is higher than, to be added in ball grinder, ball milling is added for gram molybdenum disulfide powder
After pearl, ball milling 20 hours, obtains viscous paste under the conditions of 300 revs/min；
(2) after diluting viscous paste obtained in step (1) with 480 ml deionized waters, stirring obtains curing in 30 minutes
Molybdenum dispersion liquid；
(3) by dispersion liquid freeze-drying process obtained in step (2), polyethyleneglycol modified molybdenum disulfide powder is obtained；
(4) powder obtained by step (3) is annealed 1 hour in 700 DEG C of nitrogen atmosphere, obtains pure molybdenum disulfide powder.It moves back
Heating rate during fire is 10 DEG C/min, and initial temperature is room temperature；After annealing, sample is naturally cold in nitrogen atmosphere
But.
Embodiment 4
(1) 10 grams of polyethylene glycol are dissolved under agitation in 25 ml deionized waters, until completely dissolved, by solution and 20
(100 microns of tungsten disulfide feedstock Particle size, 95%) content, which is higher than, to be added in ball grinder, ball milling is added for gram tungsten disulfide powder
After pearl, ball milling 20 hours, obtains viscous paste under the conditions of 600 revs/min；
(2) after diluting viscous paste obtained in step (1) with 480 ml deionized waters, stirring obtains curing in 30 minutes
Tungsten dispersion liquid；
(3) by dispersion liquid freeze-drying process obtained in step (2), polyethyleneglycol modified tungsten disulfide powder is obtained；
(4) powder obtained by step (3) is annealed 1 hour in 700 DEG C of nitrogen atmosphere, obtains pure tungsten disulfide powder.It moves back
Heating rate during fire is 10 DEG C/min, and initial temperature is room temperature；After annealing, sample is naturally cold in nitrogen atmosphere
But.
Embodiment 5
(1) 10 grams of polyvinylpyrrolidones are dissolved under agitation in 25 milliliters of ethylene glycol, until completely dissolved, by solution
(50 nanometers of molybdenum disulfide feedstock Particle size, 95%) content, which is higher than, to be added in ball grinder, ball is added with 20 grams of molybdenum disulfide powders
After grinding pearl, ball milling 20 hours, obtains viscous paste under the conditions of 150 revs/min；
(2) after diluting viscous paste obtained in step (1) with 480 milliliters of ethylene glycol, stirring obtains molybdenum disulfide in 30 minutes
Dispersion liquid；
(3) by dispersion liquid spray drying treatment obtained in step (2), polyvinyl pyrrolidon modified molybdenum disulphide powder is obtained
Body；
(4) powder obtained by step (3) is annealed 1 hour in 700 DEG C of nitrogen atmosphere, obtains pure molybdenum disulfide powder.It moves back
Heating rate during fire is 10 DEG C/min, and initial temperature is room temperature；After annealing, sample is naturally cold in nitrogen atmosphere
But.
Embodiment 6
(1) 10 grams of polyvinylpyrrolidones are dissolved under agitation in 25 milliliters of ethylene glycol, until completely dissolved, by solution
(50 nanometers of tungsten disulfide feedstock Particle size, 95%) content, which is higher than, to be added in ball grinder, ball is added with 20 grams of tungsten disulfide powders
After grinding pearl, ball milling 20 hours, obtains viscous paste under the conditions of 150 revs/min；
(2) after diluting viscous paste obtained in step (1) with 480 milliliters of ethylene glycol, stirring obtains tungsten disulfide in 30 minutes
Dispersion liquid；
(3) by dispersion liquid spray drying treatment obtained in step (2), polyvinyl pyrrolidon modified curing tungsten powder is obtained
Body；
(4) powder obtained by step (3) is annealed 1 hour in 700 DEG C of nitrogen atmosphere, obtains pure graphene powder.Annealing
Heating rate in the process is 10 DEG C/min, and initial temperature is room temperature；After annealing, sample is naturally cold in nitrogen atmosphere
But.
Embodiment 7
(1) 10 grams of polyvinyl alcohol are dissolved under agitation in 25 ml deionized waters, until completely dissolved, by solution and 20
(100 microns of molybdenum disulfide feedstock Particle size, 95%) content, which is higher than, to be added in sand mill, mill pearl is added for gram molybdenum disulfide powder
Afterwards, ball milling 20 hours under the conditions of 1600 revs/min, viscous paste is obtained；
(2) after diluting viscous paste obtained in step (1) with 480 ml deionized waters, stirring obtains curing in 30 minutes
Molybdenum dispersion liquid；
(3) dispersion obtained in step (2) is dried with super critical CO 2 technology, obtains the two of polyvinyl alcohol modification
Molybdenum sulfide powder；
(4) powder obtained by (3) is annealed 1 hour in 700 DEG C of nitrogen atmosphere, obtains pure molybdenum disulfide powder.It is annealed
Heating rate in journey is 10 DEG C/min, and initial temperature is room temperature；After annealing, sample natural cooling in nitrogen atmosphere.
Embodiment 8
(1) 10 grams of polyvinyl alcohol are dissolved under agitation in 25 ml deionized waters, until completely dissolved, by solution and 20
(100 microns of tungsten disulfide feedstock Particle size, 95%) content, which is higher than, to be added in sand mill, mill pearl is added for gram tungsten disulfide powder
Afterwards, ball milling 20 hours under the conditions of 1600 revs/min, viscous paste is obtained；
(2) after diluting viscous paste obtained in step (1) with 480 ml deionized waters, stirring obtains curing in 30 minutes
Tungsten dispersion liquid；
(3) dispersion liquid obtained in step (2) is dried with super critical CO 2 technology, obtains polyvinyl alcohol modification
Tungsten disulfide powder；
(4) powder obtained by step (3) is annealed 1 hour in 700 DEG C of nitrogen atmosphere, obtains pure tungsten disulfide powder.It moves back
Heating rate during fire is 10 DEG C/min, and initial temperature is room temperature；After annealing, sample is naturally cold in nitrogen atmosphere
But.
Embodiment 9
(1) 10 grams of polyethylene glycol are dissolved under agitation in 25 milliliters of N-Methyl pyrrolidones, it until completely dissolved, will
(500 nanometers of molybdenum disulfide particles size, 95%) content, which is higher than, to be added in ball grinder, be added for solution and 20 grams of molybdenum disulfide powders
After ball milling pearl, ball milling 20 hours, obtains viscous paste under the conditions of 150 revs/min；
(2) after diluting viscous paste obtained in step (1) with 480 milliliters of N-Methyl pyrrolidones, stirring obtains for 30 minutes
Molybdenum disulfide dispersion liquid；
(3) by dispersion liquid spray drying treatment obtained in step (2), polyethyleneglycol modified molybdenum disulfide powder is obtained；
(4) powder obtained by step (3) is annealed 1 hour in 700 DEG C of nitrogen atmosphere, obtains pure molybdenum disulfide powder.It moves back
Heating rate during fire is 10 DEG C/min, and initial temperature is room temperature；After annealing, sample is naturally cold in nitrogen atmosphere
But.
Embodiment 10
(1) 10 grams of polyethylene glycol are dissolved under agitation in 25 milliliters of N-Methyl pyrrolidones, it until completely dissolved, will be molten
(500 nanometers of tungsten disulfide feedstock Particle size, 95%) content, which is higher than, to be added in sand mill, add for liquid and 20 grams of tungsten disulfide powders
Enter after grinding pearl, ball milling 30 hours, obtains viscous paste under the conditions of 150 revs/min；
(2) after diluting viscous paste obtained in step (1) with 480 milliliters of N-Methyl pyrrolidones, stirring obtains for 30 minutes
Tungsten disulfide dispersion liquid；
(3) dispersion liquid obtained in step (2) is freeze-dried spray to be dried, obtains polyethyleneglycol modified curing tungsten powder
Body；
(4) powder obtained by step (3) is annealed 1 hour in 700 DEG C of nitrogen atmosphere, obtains pure tungsten disulfide powder.It moves back
Heating rate during fire is 10 DEG C/min, and initial temperature is room temperature；After annealing, sample is naturally cold in nitrogen atmosphere
But.
Claims (7)
1. a kind of ultra-high throughput stripping means of transient metal sulfide, it is characterised in that specific step is as follows:
(1) transient metal sulfide powder is added in the aqueous solution containing auxiliary agent, after mixing evenly, passes through ball mill or sand
Mill mechanical effect, forms viscous paste；The described transient metal sulfide removing concentration be removing concentration be greater than 200 milligrams/
Milliliter, reaches as high as 600 mg/mls；Auxiliary dosage is 0.1-2 times of transient metal sulfide powder quality；
(2) the viscous paste water or corresponding organic solvent diluting obtained step (1) stirs 30 minutes and forms stable mistake
Cross metal sulfide dispersion liquid；The transient metal sulfide removing concentration is that removing concentration is greater than 200 mg/mls, most
High reachable 600 mg/mls；
(3) place is dried in the viscous paste that step (1) obtains or the transient metal sulfide dispersion liquid that step (2) obtains
Reason, obtains addition agent modified transient metal sulfide powder；
(4) product for obtaining step (3) high-temperature process under inert gas or vacuum condition, obtains pure transient metal sulfide
Powder.
2. a kind of ultra-high throughput stripping means of transient metal sulfide according to claim 1, it is characterised in that step
(1) transient metal sulfide described in includes molybdenum disulfide or tungsten disulfide, and raw materials size is 50 nanometers -100 microns.
3. a kind of ultra-high throughput stripping means of transient metal sulfide according to claim 1, it is characterised in that step
(1) auxiliary agent includes any in polyvinylpyrrolidone, polyethylene glycol or polyvinyl alcohol.
4. a kind of ultra-high throughput stripping means of transient metal sulfide according to claim 1, it is characterised in that step
(2) organic solvent described in includes ethyl alcohol, methanol, N, any in N-dimethylformamide, N-Methyl pyrrolidone or ethylene glycol
Kind.
5. a kind of ultra-high throughput stripping means of transient metal sulfide according to claim 1, it is characterised in that step
(1) the sand mill revolving speed described in is 150-1600 revs/min, and it is 0.5-24 hours that the time, which is sanded,；Drum's speed of rotation is 150-
600 revs/min, Ball-milling Time is 1-24 hours.
6. a kind of ultra-high throughput stripping means of transient metal sulfide according to claim 1, it is characterised in that step
(3) described be dried includes being spray-dried, surpassing and close in dry carbon dioxide, freeze-drying, vacuum drying or forced air drying
It is any.
7. a kind of ultra-high throughput stripping means of transient metal sulfide according to claim 1, it is characterised in that step
(4) inert gas described in includes nitrogen or argon gas.
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