CN104973593A - Stripping method of stratified materials - Google Patents
Stripping method of stratified materials Download PDFInfo
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- CN104973593A CN104973593A CN201510340731.5A CN201510340731A CN104973593A CN 104973593 A CN104973593 A CN 104973593A CN 201510340731 A CN201510340731 A CN 201510340731A CN 104973593 A CN104973593 A CN 104973593A
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Abstract
The invention discloses a stripping method of stratified materials. The stripping method comprises the following steps of: weighing 30-70% of stratified materials, 0.2-5% of an organic intercalation agent, and the balance of a solvent, and mixing and stirring the weighed stratified materials, the weighed organic intercalation agent and the weighed solvent so as to obtain paste; placing the paste in a closed container, and performing static steeping; heating the steeped paste under the condition of continuously stirring, filtering the paste, washing the filtered paste, drying the washed paste so as to obtain a filter cake; placing 10-50% of filter cake, 0.5-30% of an inorganic intercalation agent, and the balance of a solvent into a closed container, uniformly mixing the filter cake, the inorganic intercalation agent and the solvent so as to obtain paste; performing static steeping; heating the closed container with the paste under the condition of 50-200 DEG C for 2-8h; cooling the heated closed container with the paste to room temperature; performing repeated heating and cooling; performing filtering; performing cleaning so as to obtain a secondary filter cake and a filtrate agent; adding the secondary filter cake and the filtrate agent in the solvent for ultrasonic stripping so as to obtain a dispersion liquid; filtering the dispersion liquid; washing the filtered dispersion liquid with deionized water; and performing vacuum drying so as to obtain the stratified materials. The stripping method disclosed by the invention solves the problems that the prior art for preparing the two dimensional crystal materials is low in efficiency, small in yield, high in environmental pollution, and the like. Defects and impurities are not led in the two-dimensional crystal materials.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, relate to a kind of stratified material stripping means.
Background technology
Take Graphene as the two-dimensional atomic crystal of representative be a class type material, system is rich and varied, and structure is unique, has contained the abundant and physicochemical property of novelty, has had broad application prospects in fields such as electronics, information, the energy.In recent years, two-dimensional atomic crystal material particularly Graphene research has achieved a series of impressive progress, new results, new discovery emerge in an endless stream, but the preparation of two-dimensional atomic crystal material is still in the starting stage at present on the whole, face a lot of opportunities and challenges, extensive, the low cost of New Two Dimensional atomic crystal material system, controlledly synthesis and preparation are significant.
Stratified material is the three-dimensional structure of being piled up by weak force by two-dimensional slice, and its Typical Representative is the graphite piled up by countless single-layer graphene, also there is other stratified material a lot of simultaneously, as: layer silicate mineral, mica, BN, WS
2, MoS
2, MoSe
2, GaTe, Bi
2se
3, TaSe
2, MnO
2, V
2o
5deng.Because these materials show excellent electricity, optics, mechanics and electrochemical properties, in the past in 10 years, many preparation methods have been developed in order to obtain the single sheet of these stratified materials, wherein, most important, have the method for application prospect to be liquid phase stripping means most.Liquid phase stripping means not only generates a large amount of nano flakes in the solution, may be used for preparing film and matrix material, and its process is simple, low for equipment requirements, has potential industrial prospect.But liquid phase stripping means will carry out being oxidized usually before stripping, ion insertion or ion-exchange, then peel off in the solution and obtain monolayer material, because the generation of oxidation, ion insertion or ion exchange process, inevitably on the two dimensional crystal material of preparation, produce defect or impurity, and then affect physics, the chemical property of two dimensional crystal material.Therefore be necessary to develop a kind of can simple, effective stripped laminar material, not only not in two dimensional crystal material, do not introduce the method for defect and impurity.
Summary of the invention
The object of this invention is to provide a kind of stratified material stripping means, low to solve the efficiency that currently available technology prepared existing for two dimensional crystal material, output is little, high cost, the problems such as high environmental pollution.Meanwhile, in two dimensional crystal material, do not introduce defect and impurity again, this preparation method is simple, and less energy-consumption is low for equipment requirements, pollution-free, and suitable extensive preparation, is with a wide range of applications.
The technical solution adopted in the present invention is, a kind of stratified material stripping means, specifically carries out according to following steps:
Step 1,
According to mass percent, take the stratified material of 30-70%, 0.2-5% organic intercalation agent, all the other for solvent, stratified material, organic intercalation agent and stirring solvent are mixed, obtain slurry, slurry is put into encloses container, static dipping 2-48h;
Step 2,
Slurry step 1 obtained heats 2-5h under constantly stirring, heating 50-200 DEG C, by slurries filtration, washing, drying, and the filter cake obtained;
Step 3,
According to mass percent, by the filter cake of 10-50%, inorganic intercalated dose of 0.5-30%, all the other are solvent, load encloses container, mix furnishing slurry, static dipping 5 ~ 32h;
Step 4,
The encloses container heating 2-8h of slurry will be housed under 50-200 DEG C of condition, and be cooled to room temperature, repeatedly heat, cool 3-5 time;
Step 5,
By slurries filtration cooled in step 4, cleaning 3-5 time, obtain secondary filter cake and filtrate, circulation or recovery filtrate in inorganic intercalated dose;
Step 6,
Join in solvent by the secondary filter cake obtained in step 5, mass ratio shared by secondary filter cake is 20-5%, ultrasonic stripping 0.5-12h, obtains individual layer and multilayer chip dispersion of materials liquid;
Step 7,
Filtered by the dispersion liquid of individual layer and multilayer chip material, by washed with de-ionized water 3-5 time, vacuum-drying, obtains individual layer and multilayer chip material solid powder.
Preferably, stratified material is graphite, BN, WS
2, TbSe
2, TaSe
2, MnO
2, V
2o
5, polynite, kaolinite, mica powder, MoX
2, GaX, InX, X=S, Se or Te.
Preferably, graphite is one or more mixtures of synthetic graphite, aphanitic graphite, crystalline flake graphite.
Preferably, organic intercalation agent is ammonium formiate, methane amide, ammonium acetate, ethanamide, ammonium benzoate, benzamide, phthalic acid ammonium, benzenedicarboxamide, phthalic imidine, N-MU, N, N-dimethyl urea, N-ethyl carbamide, N, N-diethyl urea, CO (NH
2)
2, biuret, thiocarbamide one or more mixtures.
Preferably, phthalic acid ammonium is one or more mixtures of ammonium phthalate, m-phthalic acid ammonium, terephthalic acid ammonium.
Preferably, benzenedicarboxamide is one or more mixtures of phthalic diamide, m-phthalic acid acid amides, terephthalic acid acid amides.
Preferably, solvent is one or both the mixture in water, methyl alcohol, ethanol, Virahol, tetrahydrofuran (THF), acetone, N, N-dimethyl formamide, dimethyl sulfoxide (DMSO), N-methyl-2-pyrrolidone.
Preferably, inorganic intercalated dose is NH
4cl, NH
4nO
3, NaNO
3,hNO
3, (NH
4)
2sO
4, (NH
4)
2s
2o
8, NH
4sCN, (NH
4)
2cO
3, NH
4hCO
3, (NH
4)
3pO
4, NH
4h
2pO
4, (NH
4)
2hPO
4, ammonium polyphosphate, H
2o
2, SPC-D, antihypo one or more mixtures.
The invention has the beneficial effects as follows:
1. the intercalator raw material that the inventive method adopts is general chemical raw material, and price is low, capable of circulation or recycling.
2. the individual layer prepared by the inventive method stripped laminar material and multilayer two-dimension crystalline material no significant defect, do not introduce impurity in individual layer and multilayer two-dimension crystalline material.
3. the inventive method technique is simple, and equipment is simple, and mild condition, cost is low.
4. the inventive method does not produce the three wastes, environmental friendliness.
Utilize preparation method of the present invention can obtain single or multiple lift two dimensional crystal material, as: Graphene, nano-graphene sheet, individual layer molybdenumdisulphide etc.For the purification of natural graphite ore deposit and molybdenum glance, natural graphite through repeatedly intercalation, peel off and can obtain individual layer and multi-layer graphene nanometer sheet, high-carbon graphite and high purity graphite, molybdenum glance through repeatedly intercalation, peel off and can obtain individual layer and multilayer MoS
2with the MoS of different purity
2.Therefore, by the inventive method, natural graphite and molybdenum glance are purified, all in the interest field of application claims protection.
Embodiment
A kind of stratified material stripping means, stratified material, intercalator and solvent is even, and obtain slurries, dipping, heating, ultrasonic stripping, obtain individual layer and multilayer two-dimension material.
Specifically carry out according to following steps:
Step 1,
According to mass percent, take the stratified material of 30-70%, 0.2-5% organic intercalation agent, all the other for solvent, stratified material, organic intercalation agent and stirring solvent are mixed, obtain slurry, slurry is put into encloses container, static dipping 2-48h;
Wherein, stratified material is graphite, BN, WS
2, TbSe
2, TaSe
2, MnO
2, V
2o
5, polynite, kaolinite, mica powder, MoX
2, GaX, InX, X=S, Se or Te; In particular, graphite is one or more mixtures of synthetic graphite, aphanitic graphite, crystalline flake graphite;
Organic intercalation agent is ammonium formiate, methane amide, ammonium acetate, ethanamide, ammonium benzoate, benzamide, phthalic acid ammonium, benzenedicarboxamide, phthalic imidine, N-MU, N, N-dimethyl urea, N-ethyl carbamide, N, N-diethyl urea, CO (NH
2)
2, biuret, thiocarbamide one or more mixtures; In particular, phthalic acid ammonium is one or more mixtures of ammonium phthalate, m-phthalic acid ammonium, terephthalic acid ammonium; Benzenedicarboxamide is one or more mixtures of phthalic diamide, m-phthalic acid acid amides, terephthalic acid acid amides.
Solvent is one or both the mixture in water, methyl alcohol, ethanol, Virahol, tetrahydrofuran (THF), acetone, N, N-dimethyl formamide, dimethyl sulfoxide (DMSO), N-methyl-2-pyrrolidone;
Step 2,
Slurry step 1 obtained heats 2-5h under constantly stirring, heating 50-200 DEG C, by slurries filtration, washing, drying, and the filter cake obtained, in filtrate, organic intercalation agent reclaims or recycles;
Step 3,
According to mass percent, by the filter cake of 10-50%, inorganic intercalated dose of 0.5-30%, all the other are solvent, load encloses container, mix furnishing slurry, static dipping 5 ~ 32h;
Wherein, inorganic intercalated dose is NH
4cl, NH
4nO
3, NaNO
3,hNO
3, (NH
4)
2sO
4, (NH
4)
2s
2o
8, NH
4sCN, (NH
4)
2cO
3, NH
4hCO
3, (NH
4)
3pO
4, NH
4h
2pO
4, (NH
4)
2hPO
4, ammonium polyphosphate, H
2o
2, SPC-D, antihypo one or more mixtures.
Step 4,
The encloses container heating 2-8h of slurry will be housed under 50-200 DEG C of condition, and be cooled to room temperature, repeatedly heat, cool 3-5 time;
Step 5,
By slurries filtration cooled in step 4, cleaning 3-5 time, obtain secondary filter cake and filtrate, circulation or recovery filtrate in inorganic intercalated dose;
Step 6,
Join in solvent by the secondary filter cake obtained in step 5, wherein mass ratio shared by filter cake is 20-5%, ultrasonic stripping 0.5-12h, obtains individual layer and multilayer chip dispersion of materials liquid;
Solvent is one or both the mixture in water, methyl alcohol, ethanol, Virahol, tetrahydrofuran (THF), acetone, N, N-dimethyl formamide, dimethyl sulfoxide (DMSO), N-methyl-2-pyrrolidone.
Step 7,
Filtered by the dispersion liquid of individual layer and multilayer chip material, by washed with de-ionized water 3-5 time, vacuum-drying, obtains individual layer and multilayer chip material solid powder (can again disperse in a solvent).
Embodiment 1
According to mass percent, take the stratified material of 30%, 0.2% organic intercalation agent, all the other for water, stratified material, organic intercalation agent and stirring solvent are mixed, obtain slurry, slurry is put into encloses container, static dipping 2h; Stratified material is graphite; Organic intercalation agent is ammonium formiate.By the slurry that obtains at 50 DEG C, and heat 5h under constantly stirring, by slurries filtration, washing, drying, the filter cake obtained; According to mass percent, by the filter cake of 10%, 0.5% inorganic intercalated dose, all the other are water, load encloses container, mix furnishing slurry, static dipping 5h; Inorganic intercalated dose is NH
4cl.The encloses container heating 8h of slurry will be housed under 50 DEG C of conditions, and be cooled to room temperature, repeatedly heat, cool 3 times; By slurries filtration, cleaning 3 times, obtain secondary filter cake and filtrate; Be added to the water by secondary filter cake, mass ratio shared by filter cake is 20%, ultrasonic stripping 0.5h, obtains individual layer and multilayer chip dispersion of materials liquid; Filtered by the dispersion liquid of individual layer and multilayer chip material, by washed with de-ionized water 3 times, vacuum-drying, obtains individual layer and multilayer chip material solid powder.
Embodiment 2
According to mass percent, take the stratified material of 70%, 5% organic intercalation agent, all the other for methyl alcohol, stratified material, organic intercalation agent and stirring solvent are mixed, obtain slurry, slurry is put into encloses container, static dipping 48h; Stratified material is BN; Organic intercalation agent is ammonium phthalate.By the slurry that obtains at 200 DEG C, and heat 5h under constantly stirring, by slurries filtration, washing, drying, the filter cake obtained, in filtrate, organic intercalation agent reclaims or recycles; According to mass percent, by the filter cake of 50%, 30% inorganic intercalated dose, all the other are methyl alcohol, load encloses container, mix furnishing slurry, static dipping 32h; Inorganic intercalated dose is NH
4nO
3.The encloses container heating 2h of slurry will be housed under 200 DEG C of conditions, and be cooled to room temperature, repeatedly heat, cool 5 times; By slurries filtration, cleaning 5 times, obtain secondary filter cake and filtrate; Join in methyl alcohol by secondary filter cake, mass ratio shared by filter cake is 5%, ultrasonic stripping 12h, obtains individual layer and multilayer chip dispersion of materials liquid; Filtered by the dispersion liquid of individual layer and multilayer chip material, by washed with de-ionized water 5 times, vacuum-drying, obtains individual layer and multilayer chip material solid powder.
Embodiment 3
According to mass percent, take the stratified material of 50%, 3% organic intercalation agent, all the other for ethanol, stratified material, organic intercalation agent and stirring solvent are mixed, obtain slurry, slurry is put into encloses container, static dipping 24h; Stratified material is polynite; Organic intercalation agent is phthalic diamide.By the slurry that obtains at 100 DEG C, and heat 5h under constantly stirring, by slurries filtration, washing, drying, the filter cake obtained; According to mass percent, by the filter cake of 30%, 10% inorganic intercalated dose, all the other are ethanol, load encloses container, mix furnishing slurry, static dipping 12h; Inorganic intercalated dose is NaNO
3.The encloses container heating 5h of slurry will be housed under 100 DEG C of conditions, and be cooled to room temperature, repeatedly heat, cool 4 times; By slurries filtration, cleaning 4 times, obtain secondary filter cake and filtrate; Join in ethanol by secondary filter cake, mass ratio shared by filter cake is 10%, ultrasonic stripping 6h, obtains individual layer and multilayer chip dispersion of materials liquid; Filtered by the dispersion liquid of individual layer and multilayer chip material, by washed with de-ionized water 4 times, vacuum-drying, obtains individual layer and multilayer chip material solid powder.
Embodiment 4
According to mass percent, take the aphanitic graphite (carbon content: 43.2%), the benzamide of 4%, all the other are tetrahydrofuran (THF), are uniformly mixed, obtain slurry, slurry is put into encloses container, static dipping 24h of 40%; By the slurry that obtains at 80 DEG C, and heat 5h under constantly stirring, by slurries filtration, washing, drying, the filter cake obtained; According to mass percent, by the filter cake of the 20%, (NH of 15%
4)
2sO
4, all the other are tetrahydrofuran (THF), load encloses container, mix furnishing slurry, static dipping 24h; The encloses container heating 3h of slurry will be housed under 150 DEG C of conditions, and be cooled to room temperature, repeatedly heat, cool 4 times; By slurries filtration, cleaning 4 times, obtain secondary filter cake and filtrate; Join in tetrahydrofuran (THF) by secondary filter cake, mass ratio shared by filter cake is 10%, ultrasonic stripping 10h, obtains individual layer and multilayer chip dispersion of materials liquid; Filtered by the dispersion liquid of individual layer and multilayer chip material, by washed with de-ionized water 5 times, vacuum-drying, obtains individual layer and multilayer chip material solid powder.
Embodiment 5
According to mass percent, take the molybdenumdisulphide of 30%, 5% biuret, all the other for water, be uniformly mixed, obtain slurry, slurry is put into encloses container, static dipping 48h; By the slurry that obtains at 200 DEG C, and heat 4h under constantly stirring, by slurries filtration, washing, drying, the filter cake obtained; According to mass percent, by the filter cake of 50%, the H of 30%
2o
2, all the other are water, load encloses container, mix furnishing slurry, static dipping 32h; The encloses container heating 8h of slurry will be housed under 200 DEG C of conditions, and be cooled to room temperature, repeatedly heat, cool 5 times; By slurries filtration, cleaning 5 times, obtain secondary filter cake and filtrate, circulation or to reclaim in filtrate inorganic intercalated dose; Be added to the water by secondary filter cake, mass ratio shared by filter cake is 8%, ultrasonic stripping 12h, obtains individual layer and multilayer chip dispersion of materials liquid; Filtered by the dispersion liquid of individual layer and multilayer chip material, by washed with de-ionized water 5 times, vacuum-drying, obtains individual layer and multilayer chip material solid powder.
Claims (8)
1. a stratified material stripping means, is characterized in that, specifically carries out according to following steps:
Step 1,
According to mass percent, take the stratified material of 30-70%, 0.2-5% organic intercalation agent, all the other for solvent, stratified material, organic intercalation agent and stirring solvent are mixed, obtain slurry, slurry is put into encloses container, static dipping 2-48h;
Step 2,
Slurry step 1 obtained heats 2-5h under constantly stirring, heating 50-200 DEG C, by slurries filtration, washing, drying, and the filter cake obtained;
Step 3,
According to mass percent, by the filter cake of 10-50%, inorganic intercalated dose of 0.5-30%, all the other are solvent, load encloses container, mix furnishing slurry, static dipping 5 ~ 32h;
Step 4,
The encloses container heating 2-8h of slurry will be housed under 50-200 DEG C of condition, and be cooled to room temperature, repeatedly heat, cool 3-5 time;
Step 5,
By slurries filtration cooled in step 4, cleaning 3-5 time, obtain secondary filter cake and filtrate, circulation or recovery filtrate in inorganic intercalated dose;
Step 6,
Join in solvent by the secondary filter cake obtained in step 5, wherein mass ratio shared by secondary filter cake is 20-5%, ultrasonic stripping 0.5-12h, obtains individual layer and multilayer chip dispersion of materials liquid;
Step 7,
Filtered by the dispersion liquid of individual layer and multilayer chip material, by washed with de-ionized water 3-5 time, vacuum-drying, obtains individual layer and multilayer chip material solid powder.
2. a kind of stratified material stripping means according to claim 1, is characterized in that, layered material is graphite, BN, WS
2, TbSe
2, TaSe
2, MnO
2, V
2o
5, polynite, kaolinite, mica powder, MoX
2, GaX, InX, X=S, Se or Te.
3. a kind of stratified material stripping means according to claim 2, is characterized in that, described graphite is one or more mixtures of synthetic graphite, aphanitic graphite, crystalline flake graphite.
4. a kind of stratified material stripping means according to claim 1, it is characterized in that, described organic intercalation agent is ammonium formiate, methane amide, ammonium acetate, ethanamide, ammonium benzoate, benzamide, phthalic acid ammonium, benzenedicarboxamide, phthalic imidine, N-MU, N, N-dimethyl urea, N-ethyl carbamide, N, N-diethyl urea, CO (NH
2)
2, biuret, thiocarbamide one or more mixtures.
5. a kind of stratified material stripping means according to claim 4, is characterized in that, described phthalic acid ammonium is one or more mixtures of ammonium phthalate, m-phthalic acid ammonium, terephthalic acid ammonium.
6. a kind of stratified material stripping means according to claim 4, is characterized in that, described benzenedicarboxamide is one or more mixtures of phthalic diamide, m-phthalic acid acid amides, terephthalic acid acid amides.
7. a kind of stratified material stripping means according to claim 1, it is characterized in that, described solvent is one or both the mixture in water, methyl alcohol, ethanol, Virahol, tetrahydrofuran (THF), acetone, N, N-dimethyl formamide, dimethyl sulfoxide (DMSO), N-methyl-2-pyrrolidone.
8. a kind of stratified material stripping means according to claim 1, is characterized in that, described inorganic intercalated dose is NH
4cl, NH
4nO
3, NaNO
3,hNO
3, (NH
4)
2sO
4, (NH
4)
2s
2o
8, NH
4sCN, (NH
4)
2cO
3, NH
4hCO
3, (NH
4)
3pO
4, NH
4h
2pO
4, (NH
4)
2hPO
4, ammonium polyphosphate, H
2o
2, SPC-D, antihypo one or more mixtures.
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