CN109368623A - A kind of nano metal intercalated graphite alkene preparation method - Google Patents
A kind of nano metal intercalated graphite alkene preparation method Download PDFInfo
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- CN109368623A CN109368623A CN201811101758.9A CN201811101758A CN109368623A CN 109368623 A CN109368623 A CN 109368623A CN 201811101758 A CN201811101758 A CN 201811101758A CN 109368623 A CN109368623 A CN 109368623A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/30—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
Abstract
Disclosed herein is a kind of preparation methods of nano metal graphene intercalation, the following steps are included: expanded graphite, which is carried out high temperature and pressure grinding, obtains few layer graphene, then it is added under hydrothermal reaction kettle high temperature with metal ion ammonium salt complex solution and reacts certain time, following reaction object washing removal surface residual ion, final powder carries out high-temperature calcination, and interlayer metal ion, which is finally reduced, generates nano metal intercalated graphite alkene.This technology is not necessarily to redox reagent, and pollution-free waste water generates, environmentally protective.Graphene is few through physical method processability defect, and nano metal finally in interlayer in-situ preparation, occurs crystal with graphene and couples, antibacterial and catalysis are significantly improved.
Description
Technical field
The present invention relates to a kind of preparation method of nano metal intercalated graphite alkene, in particular to a kind of nano silver graphene is inserted
The preparation method of layer.
Background technique
Graphene (Graphene) is a kind of two dimension for forming hexangle type in honeycomb lattice with sp2 hybridized orbit by carbon atom
Carbon nanomaterial.The method of the common power production of graphene be mechanical stripping method, oxidation-reduction method, SiC epitaxial growth method, it is thin
Film production method is chemical vapour deposition technique (CVD).It is domestic at present many still using backward oxidation due to cost etc.
Reduction method preparation.
The distance of graphene film interlayer expands layer actually by oxidation reaction or hydro-thermal reaction, when interlamellar spacing expands to
When 0.8nm or more, some metal ions and small molecule can penetrate into graphene film interlayer by diffusion, pass through life in situ
It can get nano metal intercalated graphite alkene at reacting.The graphene of nano material adherency relative to surface growth, nano metal
Intercalated graphite alkene has stronger quantum effect and coupling effect, can substantially reduce contact resistance and semiconductor energy gap, greatly
Light, electricity, the magnetic property of big extension nano material.Its performance is considerably beyond common graphite alkene composite material.Therefore, intercalated graphite alkene
Material is current forefront, performance one of cash material the most brilliant.
The present invention is pioneering to prepare multi-layer graphene using physical shear method, and using hydro-thermal expand layer principle infiltration metal from
Son enters interlayer, and prepares nano metal intercalated graphite alkene by subsequent high temperature calcining.Prepared composite material has excellent
Antibacterial, catalytic performance, while having both the function such as graphene physical and chemical stability, antistatic electrical property, electromagnetic wave shielding, against weather
Energy.
Summary of the invention
It is an object of the invention to the technical problem to be solved is that: using physical method preparation structure improve can mass
The nano metal intercalated graphite alkene of production.
In order to better solve above-mentioned technical problem, the technical scheme is that providing a kind of nano metal intercalated graphite
The preparation method of alkene, includes the following steps:
1, a kind of preparation method of nano metal intercalated graphite alkene, it is characterised in that include the following steps:
(1) shear at high temperature equipment high temperature THE ADIABATIC SHEAR IN is added in expanded graphite；
(2) certain density metal precursor is mixed in proportion with water, ammonium hydroxide, obtains metal complex solution；
(3) graphene powder and metal front liquid solution are mixed and added in hydrothermal reaction kettle, it after the reaction was completed will reaction
Whole liquid centrifugation, can obtain metal ion intercalation graphene.The crude product removes impurity through repeatedly washing, and highest temperature drying can obtain
Corresponding powder.
(4) above-mentioned powder, which is placed in the calcining of Muffle furnace high temperature, can be obtained nano metal intercalated graphite alkene.
2, a kind of high temperature THE ADIABATIC SHEAR IN method according to claim 1, it is characterised in that: shear temperature is 180 DEG C,
Shear velocity is that 100-1000 turns/min, and shear pressure is 20-1000 atmospheric pressure.
3, metal precursor ammonium hydroxide complex compound according to claim 2, it is characterised in that: metal precursor is to include
AgNO3, chloric acid gold, chloroplatinic acid；Metal complex GOLD FROM PLATING SOLUTION category content concn is 10-8000mg/L；Prepare metal complex solution
Process is to be added to ammonium hydroxide in metal front liquid solution with titration mode, until solution clarification.
4, graphene according to claim 3, it is characterised in that reaction process graphene and metal net content ratio
For 1:1-49:1；Hydrothermal temperature is 180 DEG C, and the reaction time is 1-6 hours；Product centrifugal speed is after reaction
5000-10000r/min, time 5-30min；Washing methods be anhydrous propanone washing → centrifugation → deionized water washing → from
The heart.
5, high-temperature calcination technique according to claim 4, it is characterised in that calcination atmosphere is nitrogen or argon gas；It forges
Burning temperature is 300-800 DEG C；Calcination time is 6-0.5h.
Technical solution of the present invention prepares few layer graphene using physical method, followed by hydro-thermal reaction by metal ion intercalation
Enter interlayer, final high temperature is calcined to obtain nano metal intercalated graphite alkene.Prepared product graphene-structured is perfect, and nano metal exists
It is grown between graphene layer, crystal height matching, collaboration coupling is strong, and antibacterial and catalytic performance are brilliant.
Compared with prior art, the invention has the advantages that
1, few layer graphene uses high temperature and pressure grinding method, solves that chemistry redox method is seriously polluted, and preparation process is multiple
The problems such as miscellaneous harshness, inefficiency.
2, few layer graphene-structured, which is directly removed by graphite physical, obtains, structurally consummate without oxidative reduction step, electricity
Have excellent performance.
3, metal ion enters interlayer by hydro-thermal reaction, calcines to have obtained nano metal intercalated graphite by subsequent high temperature
Alkene, reaction process are environmentally protective without chemical reagent such as reducing agents；Metal ion is protected in interlayer by graphene, chemical stabilization
Property is good；Metal ion can be coordinated with graphene crystal to be grown, and contacts electronics and energy gap bottom, composite material catalytic performance are mentioned
It rises.
5, nano metal intercalated graphite alkene has outstanding antibacterial and catalysis, and steady with stable physics and chemistry
It is qualitative.
Detailed description of the invention
Fig. 1 is prepared nano metal intercalated graphite alkene TEM figure provided in an embodiment of the present invention.
Specific embodiment
The content that the present invention will be specifically described below with reference to the accompanying drawings and embodiments.
Embodiment 1:
1,10g expanded graphite is added in shear at high temperature equipment, temperature is 180 DEG C, and revolving speed is 800r/min speed, shearing
Pressure is 101MPa, grinds and can get within 3 hours few layer graphene；
2,1.8g silver nitrate is added in 1000ml aqueous solution, is prepared the silver nitrate solution of 1.8g/L, is then arrived ammonia water titration
In above-mentioned solution until solution is clarified；
3,10g is lacked layer graphene to be added in the aqueous solution of above-mentioned silver nitrate, is sufficiently added in hydrothermal reaction kettle after ultrasound
Hydro-thermal reaction 3 hours；
3, above-mentioned solution 8000r/min is centrifuged 30min, and is centrifuged repeatedly the last drying of washing using acetone and water and obtains silver ion
Intercalated graphite alkene；
4, finally above-mentioned powder is added in Muffle furnace, nanometer can be obtained within high-temperature calcination 3 hours at lower 600 DEG C of nitrogen atmosphere
Silver-colored intercalated graphite alkene.
Embodiment 2:
1,10g expanded graphite is added in shear at high temperature equipment, temperature is 180 DEG C, and revolving speed is 8000r/min speed, shearing
Pressure is 101MPa, grinds and can get within 3 hours few layer graphene；
2,1.8g silver nitrate is added in 1000ml aqueous solution, is prepared the chloric acid gold solution of 1.8g/L, is then arrived ammonia water titration
In above-mentioned solution until solution is clarified；
3,10g is lacked layer graphene to be added in the aqueous solution of above-mentioned chloric acid gold, is sufficiently added in hydrothermal reaction kettle after ultrasound
Hydro-thermal reaction 3 hours；
3, above-mentioned solution 8000r/min is centrifuged 30min, and is centrifuged repeatedly the last drying of washing using acetone and water and obtains gold ion
Intercalated graphite alkene；
4, finally above-mentioned powder is added in Muffle furnace, nanometer can be obtained within high-temperature calcination 3 hours at lower 600 DEG C of nitrogen atmosphere
Golden intercalated graphite alkene.
Claims (5)
1. a kind of preparation method of nano metal intercalated graphite alkene, it is characterised in that include the following steps:
(1) shear at high temperature equipment high temperature THE ADIABATIC SHEAR IN is added in expanded graphite；
(2) certain density metal precursor is mixed in proportion with water, ammonium hydroxide, obtains metal complex solution；
(3) graphene powder and metal front liquid solution are mixed and added in hydrothermal reaction kettle, it after the reaction was completed will reaction
Whole liquid centrifugation, can obtain metal ion intercalation graphene；
The crude product removes impurity through repeatedly washing, and highest temperature drying can obtain corresponding powder；
(4) above-mentioned powder, which is placed in the calcining of Muffle furnace high temperature, can be obtained nano metal intercalated graphite alkene.
2. a kind of high temperature THE ADIABATIC SHEAR IN method according to claim 1, it is characterised in that: shear temperature is 180 DEG C, shearing
Speed is that 100-1000 turns/min, and shear pressure is 20-8000 atmospheric pressure, and shear time is 1-10 hours.
3. metal precursor ammonium hydroxide complex compound according to claim 2, it is characterised in that: metal precursor is to include
AgNO3, chloric acid gold, chloroplatinic acid；Metal complex GOLD FROM PLATING SOLUTION category content concn is 10-8000mg/L；Prepare metal complex solution
Process is to be added to ammonium hydroxide in metal front liquid solution with titration mode, until solution clarification.
4. graphene according to claim 3, it is characterised in that reaction process graphene and metal net content ratio are 1:
1-49:1；Hydrothermal temperature is 180 DEG C, and the reaction time is 1-6 hours；Product centrifugal speed is 5000- after reaction
10000r/min, time 5-30min；Washing methods is anhydrous propanone washing → centrifugation → deionized water washing → centrifugation.
5. high-temperature calcination technique according to claim 4, it is characterised in that calcination atmosphere N2Or argon gas；Calcination temperature
It is 300-800 DEG C；Calcination time is 12-0.5h.
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Cited By (4)
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| CN112010294A (en) * | 2020-09-15 | 2020-12-01 | 昆明理工大学 | Preparation method of cobalt coordination compound molecular intercalation multilayer graphene nano material |
| CN114477152A (en) * | 2021-12-30 | 2022-05-13 | 杭州电子科技大学 | Silver nanoparticle/multilayer graphene composite material and preparation method thereof |
| CN115287895A (en) * | 2022-10-09 | 2022-11-04 | 南通缘棉家纺有限公司 | Bacteriostatic mite-killing fabric based on plant fibers and preparation method thereof |
| WO2023279356A1 (en) * | 2021-07-08 | 2023-01-12 | 苏州盛魅新材料科技有限公司 | Device for manufacturing intercalated graphene antimicrobial material |
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| CN114477152A (en) * | 2021-12-30 | 2022-05-13 | 杭州电子科技大学 | Silver nanoparticle/multilayer graphene composite material and preparation method thereof |
| CN115287895A (en) * | 2022-10-09 | 2022-11-04 | 南通缘棉家纺有限公司 | Bacteriostatic mite-killing fabric based on plant fibers and preparation method thereof |
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Application publication date: 20190222 |