CN104973593B - A kind of stratified material stripping means - Google Patents
A kind of stratified material stripping means Download PDFInfo
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- CN104973593B CN104973593B CN201510340731.5A CN201510340731A CN104973593B CN 104973593 B CN104973593 B CN 104973593B CN 201510340731 A CN201510340731 A CN 201510340731A CN 104973593 B CN104973593 B CN 104973593B
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Abstract
The invention discloses a kind of stratified material stripping means, weigh 30 70% stratified material, 0.2 5% organic intercalation agent, remaining be solvent, be stirred to obtain slurry, be put into closed container, static dipping；Lower heating is stirred continuously, by slurries filtration, washing, drying, obtained filter cake；By 10 50% filter cake, inorganic intercalated dose of 0.5 30%, remaining be solvent, load closed container, it is well mixed to be tuned into slurry, static dipping；The closed container equipped with slurry is heated into 2 8h under the conditions of 50 200 DEG C, is cooled to room temperature, heats, cool down repeatedly；Filtering, cleaning, obtain secondary filter cake and filtrate agent；It is added to ultrasound stripping in solvent；Dispersion liquid is filtered, cleaned with deionized water, is dried in vacuo and produces.Solves the problems such as efficiency that currently available technology is prepared present in two dimensional crystal material is low, and yield is small, high environmental pollution.Defect and impurity is not introduced in two dimensional crystal material.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, is related to a kind of stratified material stripping means.
Background technology
Two-dimensional atomic crystal using graphene as representative is a kind of new material, and system is rich and varied, unique structure, contains
Abundant and novel physicochemical properties, have broad application prospects in fields such as electronics, information, the energy.In recent years, two
The particularly graphene research of dimension atomic crystal material has achieved a series of impressive progresses, and new results, new discovery emerge in an endless stream, but
Two-dimensional atomic crystal material is prepared still at an early stage at present on the whole, faces many opportunities and challenges, and New Two Dimensional is former
Sub- the extensive, inexpensive of crystalline material system, controlledly synthesis and prepare significant.
Stratified material is the three-dimensional structure formed by two-dimensional slice by weak force accumulation, and its Typical Representative is by countless
The graphite that single-layer graphene accumulation forms, while many other stratified materials also be present, such as：Layer silicate mineral, mica,
BN、WS2、MoS2、MoSe2、GaTe、Bi2Se3、TaSe2、MnO2、V2O5Deng.Because these materials show excellent electricity, light
, mechanics and electrochemical properties, in past 10 years, have developed many systems to obtain the single sheet of these stratified materials
Preparation Method, wherein, method that is most important, most having application prospect is liquid phase stripping means.Liquid phase stripping means is not only in the solution
Substantial amounts of nano flake is generated, can be used for preparing film and composite, and its process is simple, low for equipment requirements, tool
There is potential industrial prospect.But liquid phase stripping means will be aoxidized generally before stripping, ion insertion or ion exchange, so
Peel off in the solution afterwards and obtain monolayer material, because the generation of oxidation, ion insertion or ion exchange process, inevitably
Defect or impurity are produced on the two dimensional crystal material of preparation, and then influences the physics of two dimensional crystal material, chemical property.Therefore
Be necessary to develop it is a kind of can it is simple, be effectively peeled off stratified material, not in two dimensional crystal material but also do not introduce defect and impurity not only
Method.
The content of the invention
It is an object of the invention to provide a kind of stratified material stripping means, and two dimensional crystal is prepared to solve currently available technology
Efficiency present in material is low, and yield is small, high cost, the problems such as high environmental pollution.Meanwhile do not draw again in two dimensional crystal material
Enter defect and impurity, the preparation method is simple and easy, and low energy consumption is low for equipment requirements, pollution-free, suitable extensive preparation, tool
Have wide practical use.
The technical solution adopted in the present invention is a kind of stratified material stripping means, specifically to follow the steps below：
Step 1,
According to mass percent, weigh 30-70% stratified material, 0.2-5% organic intercalation agent, remaining be solvent,
Stratified material, organic intercalation agent and stirring solvent are well mixed, obtain slurry, slurry is put into closed container, static leaching
Stain 2-48h；
Step 2,
The slurry that step 1 obtains is being stirred continuously lower heating 2-5h, is heating 50-200 DEG C, by slurries filtration, washing, is being done
Filter cake that is dry, obtaining；
Step 3,
According to mass percent, by 10-50% filter cake, inorganic intercalated dose of 0.5-30%, remaining be solvent, load close
Container is closed, it is well mixed to be tuned into slurry, 5~32h of static dipping；
Step 4,
The closed container equipped with slurry is heated into 2-8h under the conditions of 50-200 DEG C, is cooled to room temperature, heats repeatedly, cool down 3-
5 times；
Step 5,
By the slurries filtration after being cooled down in step 4, cleaning 3-5 times, secondary filter cake and filtrate, circulation or recovery filtrate are obtained
In inorganic intercalated dose；
Step 6,
Secondary filter cake obtained by step 5 is added in solvent, mass ratio shared by secondary filter cake is 20-5%, ultrasound
0.5-12h is peeled off, obtains individual layer and multilayer chip material dispersion liquid；
Step 7,
The dispersion liquid of individual layer and multilayer chip material is filtered, cleaned 3-5 times with deionized water, is dried in vacuo, obtains list
Layer and multilayer chip material solid powder.
Preferably, stratified material is graphite, BN, WS2、TbSe2、TaSe2、MnO2、V2O5, montmorillonite, kaolinite, mica
Powder, MoX2, GaX, InX, X=S, Se or Te.
Preferably, graphite is synthetic graphite, aphanitic graphite, one or more kinds of mixtures of crystalline flake graphite.
Preferably, organic intercalation agent is ammonium formate, formamide, ammonium acetate, acetamide, ammonium benzoate, benzamide, benzene two
Ammonium formate, benzenedicarboxamide, phthalimide, N-MU, N, N-dimethyl urea, N-ethyl carbamide, N, N-diethyl
Base urea, CO (NH2)2, biuret, one or more kinds of mixtures of thiocarbamide.
Preferably, phthalic acid ammonium is ammonium phthalate, M-phthalic acid ammonium, the one or two of terephthalic acid (TPA) ammonium
Thing mixed above.
Preferably, benzenedicarboxamide be phthalic amide, M-phthalic acid acid amides, terephthalic acid (TPA) acid amides one kind or
Two or more mixtures.
Preferably, solvent be water, methanol, ethanol, isopropanol, tetrahydrofuran, acetone, N, N-dimethylformamide, diformazan
The mixture of one or both of base sulfoxide, N-methyl pyrrolidone.
Preferably, inorganic intercalated dose is NH4Cl、NH4NO3、NaNO3、HNO3、(NH4)2SO4、(NH4)2S2O8、NH4SCN、
(NH4)2CO3、NH4HCO3、(NH4)3PO4、NH4H2PO4、(NH4)2HPO4, ammonium polyphosphate, H2O2, SODIUM PERCARBONATE, potassium percarbonate
One or more kinds of mixtures.
The beneficial effects of the invention are as follows：
1. intercalator raw material is general chemical raw material used by the inventive method, price is low, is recycled or recycles.
2. individual layer and multilayer two-dimension crystalline material no significant defect prepared by the inventive method stripped laminar material, individual layer
Impurity is not introduced into in multilayer two-dimension crystalline material.
3. the inventive method technique is simple, equipment is simple, mild condition, and cost is low.
4. the inventive method does not produce the three wastes, environment-friendly.
Single or multiple lift two dimensional crystal material can be obtained using the preparation method of the present invention, such as：Graphene, nano-graphene
Piece, individual layer molybdenum disulfide etc..For the purification of native graphite ore deposit and molybdenite, native graphite can obtain through multiple intercalation, stripping
To individual layer and multi-layer graphene nanometer sheet, high-carbon graphite and high purity graphite, molybdenite can obtain individual layer through multiple intercalation, stripping
And multilayer MoS2With the MoS of different purity2.Therefore, native graphite and molybdenite are purified with the inventive method, at this
In the claimed interest field of invention.
Embodiment
A kind of stratified material stripping means, stratified material, intercalator and solvent are well mixed, and are obtained slurries, dipping, are added
Heat, ultrasound are peeled off, and obtain individual layer and multilayer two-dimension material.
Specifically follow the steps below：
Step 1,
According to mass percent, weigh 30-70% stratified material, 0.2-5% organic intercalation agent, remaining be solvent,
Stratified material, organic intercalation agent and stirring solvent are well mixed, obtain slurry, slurry is put into closed container, static leaching
Stain 2-48h；
Wherein, stratified material is graphite, BN, WS2、TbSe2、TaSe2、MnO2、V2O5, montmorillonite, kaolinite, mica powder,
MoX2, GaX, InX, X=S, Se or Te；In particular, graphite is synthetic graphite, aphanitic graphite, one kind of crystalline flake graphite
Or two or more mixtures；
Organic intercalation agent be ammonium formate, formamide, ammonium acetate, acetamide, ammonium benzoate, benzamide, phthalic acid ammonium,
Benzenedicarboxamide, phthalimide, N-MU, N, N-dimethyl urea, N-ethyl carbamide, N, N-diethyl urea, CO
(NH2)2, biuret, one or more kinds of mixtures of thiocarbamide；In particular, phthalic acid ammonium be ammonium phthalate,
One or more kinds of mixtures of M-phthalic acid ammonium, terephthalic acid (TPA) ammonium；Benzenedicarboxamide is phthalic amide, isophthalic
One or more kinds of mixtures of dioctyl phthalate acid amides, terephthalic acid (TPA) acid amides.
Solvent be water, methanol, ethanol, isopropanol, tetrahydrofuran, acetone, N, N-dimethylformamide, dimethyl sulfoxide (DMSO),
The mixture of one or both of N-methyl pyrrolidone；
Step 2,
The slurry that step 1 obtains is being stirred continuously lower heating 2-5h, is heating 50-200 DEG C, by slurries filtration, washing, is being done
Filter cake that is dry, obtaining, organic intercalation agent recovery or recycle in filtrate；
Step 3,
According to mass percent, by 10-50% filter cake, inorganic intercalated dose of 0.5-30%, remaining be solvent, load close
Container is closed, it is well mixed to be tuned into slurry, 5~32h of static dipping；
Wherein, inorganic intercalated dose is NH4Cl、NH4NO3、NaNO3、HNO3、(NH4)2SO4、(NH4)2S2O8、NH4SCN、
(NH4)2CO3、NH4HCO3、(NH4)3PO4、NH4H2PO4、(NH4)2HPO4, ammonium polyphosphate, H2O2, SODIUM PERCARBONATE, potassium percarbonate
One or more kinds of mixtures.
Step 4,
The closed container equipped with slurry is heated into 2-8h under the conditions of 50-200 DEG C, is cooled to room temperature, heats repeatedly, cool down 3-
5 times；
Step 5,
By the slurries filtration after being cooled down in step 4, cleaning 3-5 times, secondary filter cake and filtrate, circulation or recovery filtrate are obtained
In inorganic intercalated dose；
Step 6,
Secondary filter cake obtained by step 5 is added in solvent, wherein mass ratio shared by filter cake is 20-5%, ultrasound
0.5-12h is peeled off, obtains individual layer and multilayer chip material dispersion liquid；
Solvent be water, methanol, ethanol, isopropanol, tetrahydrofuran, acetone, N, N-dimethylformamide, dimethyl sulfoxide (DMSO),
The mixture of one or both of N-methyl pyrrolidone.
Step 7,
The dispersion liquid of individual layer and multilayer chip material is filtered, cleaned 3-5 times with deionized water, is dried in vacuo, obtains list
Layer and multilayer chip material solid powder (can disperse again in a solvent).
Embodiment 1
According to mass percent, weigh 30% stratified material, 0.2% organic intercalation agent, remaining be water, by stratiform material
Material, organic intercalation agent and stirring solvent are well mixed, and obtain slurry, slurry is put into closed container, static dipping 2h；Stratiform
Material is graphite；Organic intercalation agent is ammonium formate.By obtained slurry at 50 DEG C, and lower heating 5h is stirred continuously, by slurry
Filtering, washing, dry, obtained filter cake；According to mass percent, by 10% filter cake, inorganic intercalated dose of 0.5%, remaining
For water, load closed container, it is well mixed to be tuned into slurry, static dipping 5h；Inorganic intercalated dose is NH4Cl.Will under the conditions of 50 DEG C
Closed container heating 8h equipped with slurry, is cooled to room temperature, heats, cools down 3 times repeatedly；By slurries filtration, cleaning 3 times, obtain
Secondary filter cake and filtrate；Secondary filter cake is added to the water, mass ratio shared by filter cake is 20%, and ultrasound peels off 0.5h, obtains list
Layer and multilayer chip material dispersion liquid；The dispersion liquid of individual layer and multilayer chip material is filtered, cleans 3 times with deionized water, very
Sky is dried, and obtains individual layer and multilayer chip material solid powder.
Embodiment 2
According to mass percent, weigh 70% stratified material, 5% organic intercalation agent, remaining be methanol, by stratiform material
Material, organic intercalation agent and stirring solvent are well mixed, and obtain slurry, slurry is put into closed container, static dipping 48h；Layer
Shape material is BN；Organic intercalation agent is ammonium phthalate.By obtained slurry at 200 DEG C, and lower heating 5h is stirred continuously,
By slurries filtration, washing, drying, obtained filter cake, organic intercalation agent recovery or recycle in filtrate；According to quality percentage
Than, by 50% filter cake, inorganic intercalated dose of 30%, remaining be methanol, load closed container, it is well mixed to be tuned into slurry, it is quiet
Only impregnate 32h；Inorganic intercalated dose is NH4NO3.The closed container equipped with slurry is heated into 2h under the conditions of 200 DEG C, is cooled to room temperature,
Heat, cool down 5 times repeatedly；By slurries filtration, cleaning 5 times, secondary filter cake and filtrate are obtained；Secondary filter cake is added to methanol
In, mass ratio shared by filter cake is 5%, and ultrasound peels off 12h, obtains individual layer and multilayer chip material dispersion liquid；By individual layer and multilayer
The dispersion liquid filtering of flaky material, is cleaned 5 times with deionized water, is dried in vacuo, obtains individual layer and multilayer chip material solid powder
End.
Embodiment 3
According to mass percent, weigh 50% stratified material, 3% organic intercalation agent, remaining be ethanol, by stratiform material
Material, organic intercalation agent and stirring solvent are well mixed, and obtain slurry, slurry is put into closed container, static dipping 24h；Layer
Shape material is montmorillonite；Organic intercalation agent is phthalic amide.By obtained slurry at 100 DEG C, and it is stirred continuously down and adds
Hot 5h, by slurries filtration, washing, drying, obtained filter cake；According to mass percent, by 30% filter cake, 10% without the machine transplanting of rice
Layer agent, remaining be ethanol, load closed container, be well mixed be tuned into slurry, static dipping 12h；Inorganic intercalated dose is NaNO3。
The closed container equipped with slurry is heated into 5h under the conditions of 100 DEG C, is cooled to room temperature, heats, cool down 4 times repeatedly；By slurries filtration,
Cleaning 4 times, obtains secondary filter cake and filtrate；Secondary filter cake is added in ethanol, mass ratio shared by filter cake is 10%, ultrasound stripping
From 6h, individual layer and multilayer chip material dispersion liquid are obtained；The dispersion liquid of individual layer and multilayer chip material is filtered, uses deionized water
Cleaning 4 times, vacuum drying, obtains individual layer and multilayer chip material solid powder.
Embodiment 4
According to mass percent, 40% aphanitic graphite (carbon content is weighed：43.2%), 4% benzamide, remaining
For tetrahydrofuran, it is uniformly mixed, obtains slurry, slurry is put into closed container, static dipping 24h；The slurry that will be obtained
Material is stirred continuously lower heating 5h at 80 DEG C, by slurries filtration, washing, drying, obtained filter cake；According to mass percent,
By 20% filter cake, 15% (NH4)2SO4, remaining be tetrahydrofuran, load closed container, it is well mixed to be tuned into slurry, it is static
Impregnate 24h；The closed container equipped with slurry is heated into 3h under the conditions of 150 DEG C, is cooled to room temperature, heats, cool down 4 times repeatedly；Will
Slurries filtration, cleaning 4 times, obtain secondary filter cake and filtrate；Secondary filter cake is added in tetrahydrofuran, mass ratio shared by filter cake
For 10%, ultrasound peels off 10h, obtains individual layer and multilayer chip material dispersion liquid；By individual layer and the dispersion liquid of multilayer chip material
Filtering, is cleaned 5 times with deionized water, is dried in vacuo, is obtained individual layer and multilayer chip material solid powder.
Embodiment 5
According to mass percent, weigh 30% molybdenum disulfide, 5% biuret, remaining be water, be uniformly mixed,
Slurry is obtained, slurry is put into closed container, static dipping 48h；By obtained slurry at 200 DEG C, and it is stirred continuously down
Heat 4h, by slurries filtration, washing, drying, obtained filter cake；According to mass percent, by 50% filter cake, 30% H2O2、
Remaining is water, loads closed container, well mixed to be tuned into slurry, static dipping 32h；By equipped with the close of slurry under the conditions of 200 DEG C
Container heating 8h is closed, is cooled to room temperature, heats, cool down 5 times repeatedly；By slurries filtration, cleaning 5 times, secondary filter cake and filter are obtained
Inorganic intercalated dose in liquid, circulation or recovery filtrate；Secondary filter cake is added to the water, mass ratio shared by filter cake is 8%, ultrasound stripping
From 12h, individual layer and multilayer chip material dispersion liquid are obtained；The dispersion liquid of individual layer and multilayer chip material is filtered, uses deionization
Water cleans 5 times, vacuum drying, obtains individual layer and multilayer chip material solid powder.
Claims (7)
1. a kind of stratified material stripping means, it is characterised in that specifically follow the steps below：
Step 1,
According to mass percent, weigh 30-70% stratified material, 0.2-5% organic intercalation agent, remaining be solvent, by layer
Shape material, organic intercalation agent and stirring solvent are well mixed, and obtain slurry, and slurry is put into closed container, static dipping 2-
48h；The organic intercalation agent be ammonium formate, formamide, ammonium acetate, acetamide, ammonium benzoate, benzamide, phthalic acid ammonium,
Benzenedicarboxamide, phthalimide, N-MU, N, N-dimethyl urea, N-ethyl carbamide, N, N-diethyl urea, CO
(NH2)2, biuret, one or more kinds of mixtures of thiocarbamide,
Step 2,
The slurry that step 1 obtains is being stirred continuously lower heating 2-5h, is heating 50-200 DEG C, by slurries filtration, washing, drying,
Obtained filter cake；
Step 3,
According to mass percent, by 10-50% filter cake, inorganic intercalated dose of 0.5-30%, remaining be solvent, load closed appearance
Device, it is well mixed to be tuned into slurry, 5~32h of static dipping；
Step 4,
The closed container equipped with slurry is heated into 2-8h under the conditions of 50-200 DEG C, is cooled to room temperature, heats, cool down 3-5 times repeatedly；
Step 5,
By the slurries filtration after being cooled down in step 4, cleaning 3-5 times, secondary filter cake and filtrate, nothing in circulation or recovery filtrate are obtained
Machine intercalator；
Step 6,
Secondary filter cake obtained by step 5 is added in solvent, wherein mass ratio shared by secondary filter cake is 20-5%, ultrasound
0.5-12h is peeled off, obtains individual layer and multilayer chip material dispersion liquid；
Step 7,
By the dispersion liquid of individual layer and multilayer chip material filter, clean 3-5 times with deionized water, vacuum drying, obtain individual layer and
Multilayer chip material solid powder.
A kind of 2. stratified material stripping means according to claim 1, it is characterised in that layered material be graphite,
BN、WS2、TbSe2、TaSe2、MnO2、V2O5, montmorillonite, kaolinite, mica powder, MoX2, GaX, I nX, X=S, Se or Te.
A kind of 3. stratified material stripping means according to claim 2, it is characterised in that the graphite be synthetic graphite,
One or more kinds of mixtures of aphanitic graphite, crystalline flake graphite.
4. a kind of stratified material stripping means according to claim 1, it is characterised in that the phthalic acid ammonium is adjacent benzene
Dioctyl phthalate ammonium, M-phthalic acid ammonium, one or more kinds of mixtures of terephthalic acid (TPA) ammonium.
5. a kind of stratified material stripping means according to claim 1, it is characterised in that the benzenedicarboxamide is adjacent benzene
Diformamide, M-phthalic acid acid amides, one or more kinds of mixtures of terephthalic acid (TPA) acid amides.
6. a kind of stratified material stripping means according to claim 1, it is characterised in that the solvent is water, methanol, second
Alcohol, isopropanol, tetrahydrofuran, acetone, N, one kind in N-dimethylformamide, dimethyl sulfoxide (DMSO), N-methyl pyrrolidone
Or two kinds of mixture.
7. a kind of stratified material stripping means according to claim 1, it is characterised in that described inorganic intercalated dose is NH4C
l、NH4NO3、NaNO3、HNO3、(NH4)2SO4、(NH4)2S2O8、NH4SCN、(NH4)2CO3、NH4HCO3、(NH4)3PO4、NH4H2PO4、
(NH4)2HPO4, ammonium polyphosphate, H2O2, SODIUM PERCARBONATE, one or more kinds of mixtures of potassium percarbonate.
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| CN112299383B (en) * | 2019-08-01 | 2022-04-05 | 天津大学 | Method for preparing two-dimensional layered material by stripping ternary atomic crystal |
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