CN107051381A - A kind of porous graphene/active carbon compound adsorbent and preparation method thereof - Google Patents
A kind of porous graphene/active carbon compound adsorbent and preparation method thereof Download PDFInfo
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- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28069—Pore volume, e.g. total pore volume, mesopore volume, micropore volume
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Abstract
The invention discloses a kind of porous graphene/active carbon compound adsorbent and preparation method thereof.After the reaction completely of graphite and potassium permanganate, carbohydrate powder is added in the concentrated sulfuric acid, stirred, neutrality is washed with water to afterwards, carrying out high-temperature heat treatment after drying obtains.Graphene/active carbon compound adsorbent that the present invention is obtained is jointly built-up by the glycan molecule skeleton and graphene film being carbonized.Sugar can be formed in situ porous active carbon structure after being carbonized by sulfuric acid under graphene oxide cladding, sulfuric acid, which meets water very exothermic, after adding water makes loose structure further activate, dried heat treatment makes the oxy radical fast eliminating in graphene and activated carbon, pore-creating is realized in the group removing that the gas of generation is strutted in graphene interlayer structure formation micropore, activated carbon skeleton.Gained porous material of the invention has high-specific surface area, high porosity and low-density, and stability is good, available for fields such as air cleaning, water process, catalytic carrier, electrochemical materials.
Description
Technical field
The invention belongs to grapheme material field, it is related to a kind of porous graphene/active carbon compound adsorbent.
Background technology
Since extra large nurses (Andre K.Geim) of the strong K of the peace moral of Univ Manchester UK etc. prepared stone in 2004
Since black alkene material, due to its unique structure and photoelectric property, grapheme material receives extensive attention.Single-layer graphene
With many charming performances, for example:1. high intensity, Young's modulus (1,100GPa), fracture strength (125GPa);2. it is highly thermally conductive
Rate (5,000W/mK);3. high conductivity, high carrier transport rate (200,000cm2/V·s);4. high-specific surface area (count by theory
Calculation value:2,630m2/g).The especially specific surface area of superelevation so that it is received significant attention in sorbing material field.Pass through group
Graphene aerogel prepared by dress method has the pore passage structure of intercommunication, and specific surface area is big, is current graphene sorbing material
Study hotspot.But its poor mechanical property, structure is hard to keep, it is difficult to be used alone as sorbing material.
Activated carbon is the most frequently used sorbing material at present, and it has flourishing microcellular structure, huge specific surface area and excellent
Good absorption property, and resistance to acids and bases is good.Many researchers attempt activated carbon and graphene being combined in recent years.Patent
201310590113.7《A kind of preparation method of graphene modified activated carbon》It is middle that graphene and conventional wooden or stalk are lived
Property charcoal match, the activated carbon of graphene modification is obtained after high-temperature activation, with high-specific surface area, available for capacitor neck
Domain.Patent 201410330304.4《A kind of preparation method of activated carbon/graphene complex》By biomass, carboritride and
Transistion metal compound is mixed, direct in-situ generation activated carbon/graphene composite material under hot conditions, for electrochemistry neck
Domain.
The content of the invention
The purpose of the present invention is that there is provided a kind of porous graphene/active carbon compound adsorbent for existing technical deficiency
And preparation method thereof.
The purpose of the present invention is achieved through the following technical solutions:A kind of porous graphene/active carbon compound adsorbent,
Characterized in that, being made up of activated carbon and graphene, density is 0.2~0.8g/cm3, specific surface area is 500~2000m2/ g, hole
Volume is 0.3~2cm3/g。
A kind of preparation method of porous graphene/active carbon compound adsorbent, it is characterised in that comprise the following steps:
(1) graphite of 10~30 parts by weight is taken, is prepared using Hummers methods are improved in graphene oxide, preparation process, stone
Ink and concentrated sulfuric acid mass ratio are 10~30:100, obtain graphene oxide/concentrated sulfuric acid dispersion liquid after reaction completely;
(2) take the carbohydrate powder of 10~40 parts by weight to be well mixed with the water of 1~5 parts by weight, be added to step (1) and obtain
Graphene oxide/concentrated sulfuric acid dispersion liquid in, be stirred continuously, obtain viscous pastes;
(3) viscous pastes for obtaining step (2) are washed with deionized to neutrality, obtain solid material;
(4) solid material obtained step (3) is dried, and is put into tube furnace, under nitrogen atmosphere, it is warming up to 800~
1300 DEG C, 2~10h is incubated, porous graphene/active carbon compound adsorbent is obtained.
Further, the carbohydrate powder described in step (2) is xylose, sucrose, glucose, fructose, lactose, starch, fibre
One or more in dimension element.
The beneficial effects of the present invention are:The present invention directly make use of graphene oxide preparation to need to remove after terminating first
The concentrated sulfuric acid, directly by carbohydrate powder and strong sulfuric acid response, on the one hand consume the concentrated sulfuric acid unnecessary in system, it is to avoid oxidation
Cumbersome washing, centrifugal process in graphene purification process, reduce energy consumption, cost-effective, make full use of the concentrated sulfuric acid to also reduce
Environmental pollution;On the other hand, the porous carbon skeleton obtained after carbohydrate powder and strong sulfuric acid response is oxidized graphene parcel, in situ
Form composite construction.The water added in washing is brought rapidly up system and activates loose structure.Wash dried carbon/oxidation stone
Black alkene finally gives activated carbon/graphene composite adsorbent through high temperature reduction, and the oxy radical removed during high temperature reduction produces gas
Body so that strutted between graphene film and piece, obtains microcellular structure, and further pore-creating on the activated carbon so that material is whole
The pore volume increase of body.The porous adsorbent that the present invention is obtained has high-specific surface area (500~2000m2/ g), high pore volume
(0.3~2cm3/ g) and low-density (0.2~0.8g/cm3), the cladding of graphene causes material overall more resistant to corrosion, available for sky
The fields such as gas purification, water process, catalytic carrier, electrochemical material.
Embodiment
The method for preparing porous graphene/active carbon compound adsorbent comprises the following steps:
(1) graphite of 10~30 parts by weight is taken, is prepared using Hummers methods are improved in graphene oxide, preparation process, stone
Ink and concentrated sulfuric acid mass ratio are 10~30:100, obtain graphene oxide/concentrated sulfuric acid dispersion liquid after reaction completely;(2) 10~40 are taken
The carbohydrate powder of parts by weight is well mixed with the water of 1~5 parts by weight, is added to graphene oxide/concentrated sulfuric acid that step (1) is obtained
In dispersion liquid, it is stirred continuously, obtains viscous pastes.Described carbohydrate powder be xylose, sucrose, glucose, fructose, lactose,
One or more in starch, cellulose;(3) viscous pastes for obtaining step (2) are washed with deionized to neutrality, are obtained
Obtain solid material;(4) solid material for obtaining step (3) is dried, and is put into tube furnace, under nitrogen atmosphere, is warming up to 800
~1300 DEG C, 2~10h is incubated, porous graphene/active carbon compound adsorbent is obtained.
The present invention is specifically described below by embodiment, the present embodiment is served only for doing further the present invention
Bright, it is impossible to be interpreted as limiting the scope of the invention, those skilled in the art makes one according to the content of foregoing invention
A little nonessential changes and adjustment belong to protection scope of the present invention.
Embodiment 1:
(1) take the graphite of 10 parts by weight, using improve Hummers methods prepare in graphene oxide, preparation process, graphite and
Concentrated sulfuric acid mass ratio is 10:100, obtain graphene oxide/concentrated sulfuric acid dispersion liquid after reaction completely;
(2) take the sucrose of 10 parts by weight to be well mixed with the water of 1 parts by weight, be added to the graphite oxide that step (1) is obtained
In alkene/concentrated sulfuric acid dispersion liquid, it is stirred continuously, obtains viscous pastes;
(3) viscous pastes for obtaining step (2) are washed with deionized to neutrality, obtain solid material;
(4) solid material for obtaining step (3) is dried, and is put into tube furnace, under nitrogen atmosphere, is warming up to 1000
DEG C, 2h is incubated, porous graphene/active carbon compound adsorbent is obtained.
Through above step, obtained porous graphene/active carbon compound adsorbent is black foam shape, and density is 0.39g/
cm3, specific surface area is 1340m2/ g, pore volume is 1.46cm3/ g, methylenum careuleum adsorptive value is 366ml/g.
Embodiment 2:
(1) take the graphite of 25 parts by weight, using improve Hummers methods prepare in graphene oxide, preparation process, graphite and
Concentrated sulfuric acid mass ratio is 25:100, obtain graphene oxide/concentrated sulfuric acid dispersion liquid after reaction completely;
(2) take the sucrose of 10 parts by weight to be well mixed with the water of 1 parts by weight, be added to the graphite oxide that step (1) is obtained
In alkene/concentrated sulfuric acid dispersion liquid, it is stirred continuously, obtains viscous pastes;
(3) viscous pastes for obtaining step (2) are washed with deionized to neutrality, obtain solid material;
(4) solid material for obtaining step (3) is dried, and is put into tube furnace, under nitrogen atmosphere, is warming up to 1000
DEG C, 2h is incubated, porous graphene/active carbon compound adsorbent is obtained.
Through above step, obtained porous graphene/active carbon compound adsorbent is black foam shape, and density is 0.25g/
cm3, specific surface area is 1690m2/ g, pore volume is 1.12cm3/ g, methylenum careuleum adsorptive value is 391ml/g.
Embodiment 3:
(1) take the graphite of 30 parts by weight, using improve Hummers methods prepare in graphene oxide, preparation process, graphite and
Concentrated sulfuric acid mass ratio is 30:100, obtain graphene oxide/concentrated sulfuric acid dispersion liquid after reaction completely;
(2) take the sucrose of 10 parts by weight to be well mixed with the water of 1 parts by weight, be added to the graphite oxide that step (1) is obtained
In alkene/concentrated sulfuric acid dispersion liquid, it is stirred continuously, obtains viscous pastes;
(3) viscous pastes for obtaining step (2) are washed with deionized to neutrality, obtain solid material;
(4) solid material for obtaining step (3) is dried, and is put into tube furnace, under nitrogen atmosphere, is warming up to 1300
DEG C, 2h is incubated, porous graphene/active carbon compound adsorbent is obtained.
Through above step, obtained porous graphene/active carbon compound adsorbent is black foam shape, and density is 0.2g/
cm3, specific surface area is 1860m2/ g, pore volume is 1.97cm3/ g, methylenum careuleum adsorptive value is 416ml/g.
Embodiment 4:
(1) take the graphite of 10 parts by weight, using improve Hummers methods prepare in graphene oxide, preparation process, graphite and
Concentrated sulfuric acid mass ratio is 10:100, obtain graphene oxide/concentrated sulfuric acid dispersion liquid after reaction completely;
(2) take the sucrose of 20 parts by weight to be well mixed with the water of 1.5 parts by weight, be added to the oxidation stone that step (1) is obtained
In black alkene/concentrated sulfuric acid dispersion liquid, it is stirred continuously, obtains viscous pastes;
(3) viscous pastes for obtaining step (2) are washed with deionized to neutrality, obtain solid material;
(4) solid material for obtaining step (3) is dried, and is put into tube furnace, under nitrogen atmosphere, is warming up to 800 DEG C,
2h is incubated, porous graphene/active carbon compound adsorbent is obtained.
Through above step, obtained porous graphene/active carbon compound adsorbent is black foam shape, and density is 0.51g/
cm3, specific surface area is 1420m2/ g, pore volume is 1.1cm3/ g, methylenum careuleum adsorptive value is 334ml/g.
Embodiment 5:
(1) take the graphite of 10 parts by weight, using improve Hummers methods prepare in graphene oxide, preparation process, graphite and
Concentrated sulfuric acid mass ratio is 10:100, obtain graphene oxide/concentrated sulfuric acid dispersion liquid after reaction completely;
(2) take the sucrose of 30 parts by weight to be well mixed with the water of 4 parts by weight, be added to the graphite oxide that step (1) is obtained
In alkene/concentrated sulfuric acid dispersion liquid, it is stirred continuously, obtains viscous pastes;
(3) viscous pastes for obtaining step (2) are washed with deionized to neutrality, obtain solid material;
(4) solid material for obtaining step (3) is dried, and is put into tube furnace, under nitrogen atmosphere, is warming up to 800 DEG C,
2h is incubated, porous graphene/active carbon compound adsorbent is obtained.
Through above step, obtained porous graphene/active carbon compound adsorbent is black foam shape, and density is 0.68g/
cm3, specific surface area is 1150m2/ g, pore volume is 0.73cm3/ g, methylenum careuleum adsorptive value is 309ml/g.
Embodiment 6:
(1) take the graphite of 30 parts by weight, using improve Hummers methods prepare in graphene oxide, preparation process, graphite and
Concentrated sulfuric acid mass ratio is 10:100, obtain graphene oxide/concentrated sulfuric acid dispersion liquid after reaction completely;
(2) take the carbohydrate powder of 40 parts by weight to be well mixed with the water of 5 parts by weight, be added to the oxidation that step (1) is obtained
In graphene/concentrated sulfuric acid dispersion liquid, it is stirred continuously, obtains viscous pastes;
(3) viscous pastes for obtaining step (2) are washed with deionized to neutrality, obtain solid material;
(4) solid material for obtaining step (3) is dried, and is put into tube furnace, under nitrogen atmosphere, is warming up to 1300
DEG C, 2h is incubated, porous graphene/active carbon compound adsorbent is obtained.
Through above step, obtained porous graphene/active carbon compound adsorbent is black foam shape, and density is 0.79g/
cm3, specific surface area is 520m2/ g, pore volume is 0.33cm3/ g, methylenum careuleum adsorptive value is 265ml/g.
Embodiment 7:
(1) take the graphite of 10 parts by weight, using improve Hummers methods prepare in graphene oxide, preparation process, graphite and
Concentrated sulfuric acid mass ratio is 10:100, obtain graphene oxide/concentrated sulfuric acid dispersion liquid after reaction completely;
(2) take the starch of 20 parts by weight to be well mixed with the water of 4 parts by weight, be added to the graphite oxide that step (1) is obtained
In alkene/concentrated sulfuric acid dispersion liquid, it is stirred continuously, obtains viscous pastes;
(3) viscous pastes for obtaining step (2) are washed with deionized to neutrality, obtain solid material;
(4) solid material for obtaining step (3) is dried, and is put into tube furnace, under nitrogen atmosphere, is warming up to 800 DEG C,
10h is incubated, porous graphene/active carbon compound adsorbent is obtained.
Through above step, obtained porous graphene/active carbon compound adsorbent is black foam shape, and density is 0.58g/
cm3, specific surface area is 1370m2/ g, pore volume is 0.88cm3/ g, methylenum careuleum adsorptive value is 341ml/g.
Claims (3)
1. a kind of porous graphene/active carbon compound adsorbent, it is characterised in that be made up of activated carbon and graphene, density is
0.2~0.8g/cm3Left and right, specific surface area is 500~2000m2/ g, pore volume is about 0.3~2cm3/g。
2. a kind of preparation method of porous graphene/active carbon compound adsorbent, it is characterised in that comprise the following steps:
(1) take the graphite of 10~30 parts by weight, using improve Hummers methods prepare in graphene oxide, preparation process, graphite and
Concentrated sulfuric acid mass ratio is 10~30:100, obtain graphene oxide/concentrated sulfuric acid dispersion liquid after reaction completely.
(2) take the carbohydrate powder of 10~40 parts by weight to be well mixed with the water of 1~5 parts by weight, be added to the oxygen that step (1) is obtained
In graphite alkene/concentrated sulfuric acid dispersion liquid, it is stirred continuously, obtains viscous pastes.
(3) viscous pastes for obtaining step (2) are washed with deionized to neutrality, obtain solid material;
(4) solid material for obtaining step (3) is dried, and is put into tube furnace, under nitrogen atmosphere, is warming up to 800~1300
DEG C, 2~10h of insulation or so obtains porous graphene/active carbon compound adsorbent.
3. method according to claim 2, it is characterised in that the carbohydrate powder described in step (2) is xylose, sucrose,
One or more in glucose, fructose, lactose, starch, cellulose etc..
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108126661A (en) * | 2018-01-26 | 2018-06-08 | 山东星火科学技术研究院 | A kind of preparation method of graphene/absorbent charcoal composite material absorption packet |
CN108777311A (en) * | 2018-06-04 | 2018-11-09 | 东华大学 | A kind of Pd/MGN composite material and preparation methods and application with either high redox electro catalytic activity |
CN108927112A (en) * | 2018-09-21 | 2018-12-04 | 佛山皖和新能源科技有限公司 | A kind of graphene composite aerogel adsorbent |
CN109192992A (en) * | 2018-08-24 | 2019-01-11 | 东华大学 | A kind of Pd/MGF composite material and its preparation and application |
CN110844902A (en) * | 2019-11-20 | 2020-02-28 | 常州富烯科技股份有限公司 | Graphite foam and preparation method thereof |
CN110860272A (en) * | 2019-11-04 | 2020-03-06 | 南通强生石墨烯科技有限公司 | Graphene antibacterial carbon sphere and preparation method and application thereof |
CN111659346A (en) * | 2019-03-08 | 2020-09-15 | 天津大学 | Haze collecting, absorbing and converting system based on primary battery principle |
CN112547023A (en) * | 2020-12-02 | 2021-03-26 | 萝北瑞喆烯碳新材料有限公司 | Wastewater treatment agent and preparation method and application thereof |
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Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108126661A (en) * | 2018-01-26 | 2018-06-08 | 山东星火科学技术研究院 | A kind of preparation method of graphene/absorbent charcoal composite material absorption packet |
CN108777311A (en) * | 2018-06-04 | 2018-11-09 | 东华大学 | A kind of Pd/MGN composite material and preparation methods and application with either high redox electro catalytic activity |
CN108777311B (en) * | 2018-06-04 | 2021-07-02 | 东华大学 | Pd/MGN composite material with high oxidation-reduction electrocatalytic activity and preparation method and application thereof |
CN109192992A (en) * | 2018-08-24 | 2019-01-11 | 东华大学 | A kind of Pd/MGF composite material and its preparation and application |
CN108927112A (en) * | 2018-09-21 | 2018-12-04 | 佛山皖和新能源科技有限公司 | A kind of graphene composite aerogel adsorbent |
CN111659346A (en) * | 2019-03-08 | 2020-09-15 | 天津大学 | Haze collecting, absorbing and converting system based on primary battery principle |
CN110860272A (en) * | 2019-11-04 | 2020-03-06 | 南通强生石墨烯科技有限公司 | Graphene antibacterial carbon sphere and preparation method and application thereof |
CN110844902A (en) * | 2019-11-20 | 2020-02-28 | 常州富烯科技股份有限公司 | Graphite foam and preparation method thereof |
CN112547023A (en) * | 2020-12-02 | 2021-03-26 | 萝北瑞喆烯碳新材料有限公司 | Wastewater treatment agent and preparation method and application thereof |
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