CN107051381B - 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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- B01J20/28057—Surface area, e.g. B.E.T specific surface area
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- 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
- B01J20/28076—Pore volume, e.g. total pore volume, mesopore volume, micropore volume being more than 1.0 ml/g
Abstract
The invention discloses a kind of porous graphene/active carbon compound adsorbents and preparation method thereof.After graphite and potassium permanganate react completely, carbohydrate powder is added in the concentrated sulfuric acid, is stirred, neutrality is washed with water to later, carries out high-temperature heat treatment after dry and obtain.Graphene/active carbon compound adsorbent that the present invention obtains is jointly built-up by the glycan molecule skeleton and graphene film being carbonized.After being carbonized by sulfuric acid porous active carbon structure can be formed in situ under graphene oxide cladding in sugar, sulfuric acid chance water very exothermic after water is added to activate porous structure further, heat treatment after drying makes the oxygen-containing group fast eliminating in graphene and active carbon, the gas of generation struts graphene interlayer structure and forms micropore, and pore-creating is realized in the group removing in active carbon skeleton.Gained porous material of the invention has high-specific surface area, high porosity and low-density, and stability is good, can be used for the fields such as air cleaning, water process, catalytic carrier, electrochemical material.
Description
Technical field
The invention belongs to grapheme material fields, are related to a kind of porous graphene/active carbon compound adsorbent.
Background technique
Since the strong sea K nurse of the peace moral of Univ Manchester UK (Andre K.Geim) 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, such as: 1. high-intensitive, Young's modulus (1,100GPa), breaking strength (125GPa)；2. highly thermally conductive
Rate (5,000W/mK)；3. high conductivity, high carrier transport rate (200,000cm2/V·s)；4. high-specific surface area (theory meter
Calculation value: 2,630m2/g).The especially specific surface area of superelevation, so that it is received significant attention in adsorbent material field.Pass through group
The graphene aerogel of dress method preparation has the cellular structure of intercommunication, and large specific surface area is current graphene adsorbent material
Research hotspot.But its poor mechanical property, structure are hard to keep, it is difficult to be used alone as adsorbent material.
Active carbon is most common adsorbent material, has a flourishing microcellular structure, huge specific surface area and excellent
Good absorption property, and resistance to acid and alkali is good.Many researchers attempt active carbon and graphene is compound in recent years.Patent
It is in 201310590113.7 " a kind of preparation methods of graphene modified activated carbon " that graphene and conventional wooden or stalk is living
Property charcoal match, the modified active carbon of graphene is obtained after high-temperature activation, there is high-specific surface area, can be used for capacitor neck
Domain.Patent 201410330304.4 " a kind of preparation method of active carbon/graphene complex " by biomass, carboritride and
Transistion metal compound mixes, and direct in-situ generates active carbon/graphene composite material under hot conditions, leads for electrochemistry
Domain.
Summary of the invention
The purpose of the present invention is aiming at the shortcomings of the prior art, provide a kind of porous graphene/active carbon compound adsorbent
And preparation method thereof.
The purpose of the present invention is what is be achieved through the following technical solutions: a kind of porous graphene/active carbon compound adsorbent,
It is characterized in that, being made of active 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, which comprises the following steps:
(1) graphite for taking 10~30 parts by weight prepares graphene oxide using Hummers method is improved, in preparation process, stone
Ink and concentrated sulfuric acid mass ratio are 10~30:100, and graphene oxide/concentrated sulfuric acid dispersion liquid is obtained after fully reacting；
(2) it takes the carbohydrate powder of 10~40 parts by weight to be uniformly mixed with the water of 1~5 parts by weight, is added to step (1) and obtains
Graphene oxide/concentrated sulfuric acid dispersion liquid in, be stirred continuously, obtain viscous pastes；
(3) viscous pastes that step (2) obtains 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 kept the temperature, porous graphene/active carbon compound adsorbent is obtained.
Further, carbohydrate powder described in step (2) is xylose, sucrose, glucose, fructose, lactose, starch, fibre
Tie up one of element or a variety of.
The beneficial effects of the present invention are: the present invention, which is directly utilized first after prepared by graphene oxide, to be needed to remove
The concentrated sulfuric acid on the one hand consume the concentrated sulfuric acid extra in system directly by carbohydrate powder and strong sulfuric acid response, avoid oxidation
Cumbersome washing, centrifugal process in graphene purification process, reduce energy consumption, and save the cost makes 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 package, in situ
Form composite construction.The water being added in washing is brought rapidly up system and activates porous structure.Carbon/oxidation stone after washing is dry
Black alkene finally obtains active carbon/graphene composite adsorbent through high temperature reduction, and the oxygen-containing group that when high temperature reduction removes generates gas
Body obtains microcellular structure so that strutting between graphene film and piece, and further pore-creating on the activated carbon, so that material is whole
The pore volume of body increases.The porous adsorbent that the present invention obtains 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 is so that material entirety can be used for sky more resistant to corrosion
The fields such as gas purification, water process, catalytic carrier, electrochemical material.
Specific embodiment
Porous graphene/active carbon compound adsorbent method is prepared to include the following steps:
(1) graphite for taking 10~30 parts by weight prepares graphene oxide using Hummers method is improved, in preparation process, stone
Ink and concentrated sulfuric acid mass ratio are 10~30:100, and graphene oxide/concentrated sulfuric acid dispersion liquid is obtained after fully reacting；(2) 10~40 are taken
The carbohydrate powder of parts by weight is uniformly mixed with the water of 1~5 parts by weight, is added to graphene oxide/concentrated sulfuric acid that step (1) obtains
It in dispersion liquid, is stirred continuously, obtains viscous pastes.The carbohydrate powder be xylose, sucrose, glucose, fructose, lactose,
One of starch, cellulose are a variety of；(3) viscous pastes that step (2) obtains 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 kept the temperature, 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
It is bright, it should not be understood 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) graphite for taking 10 parts by weight prepares graphene oxide using Hummers method is improved, in preparation process, graphite and
Concentrated sulfuric acid mass ratio is 10:100, and graphene oxide/concentrated sulfuric acid dispersion liquid is obtained after fully reacting；
(2) it takes the sucrose of 10 parts by weight and the water of 1 parts by weight to be uniformly mixed, is added to the graphite oxide that step (1) obtains
In alkene/concentrated sulfuric acid dispersion liquid, it is stirred continuously, obtains viscous pastes；
(3) viscous pastes that step (2) obtains 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 kept the temperature, porous graphene/active carbon compound adsorbent is obtained.
Through above step, obtained porous graphene/active carbon compound adsorbent is black foam shape, density 0.39g/
cm3, specific surface area 1340m2/ g, pore volume 1.46cm3/ g, methylenum careuleum adsorptive value are 366ml/g.
Embodiment 2:
(1) graphite for taking 25 parts by weight prepares graphene oxide using Hummers method is improved, in preparation process, graphite and
Concentrated sulfuric acid mass ratio is 25:100, and graphene oxide/concentrated sulfuric acid dispersion liquid is obtained after fully reacting；
(2) it takes the sucrose of 10 parts by weight and the water of 1 parts by weight to be uniformly mixed, is added to the graphite oxide that step (1) obtains
In alkene/concentrated sulfuric acid dispersion liquid, it is stirred continuously, obtains viscous pastes；
(3) viscous pastes that step (2) obtains 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 kept the temperature, porous graphene/active carbon compound adsorbent is obtained.
Through above step, obtained porous graphene/active carbon compound adsorbent is black foam shape, density 0.25g/
cm3, specific surface area 1690m2/ g, pore volume 1.12cm3/ g, methylenum careuleum adsorptive value are 391ml/g.
Embodiment 3:
(1) graphite for taking 30 parts by weight prepares graphene oxide using Hummers method is improved, in preparation process, graphite and
Concentrated sulfuric acid mass ratio is 30:100, and graphene oxide/concentrated sulfuric acid dispersion liquid is obtained after fully reacting；
(2) it takes the sucrose of 10 parts by weight and the water of 1 parts by weight to be uniformly mixed, is added to the graphite oxide that step (1) obtains
In alkene/concentrated sulfuric acid dispersion liquid, it is stirred continuously, obtains viscous pastes；
(3) viscous pastes that step (2) obtains 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 kept the temperature, porous graphene/active carbon compound adsorbent is obtained.
Through above step, obtained porous graphene/active carbon compound adsorbent is black foam shape, density 0.2g/
cm3, specific surface area 1860m2/ g, pore volume 1.97cm3/ g, methylenum careuleum adsorptive value is 416ml/g.
Embodiment 4:
(1) graphite for taking 10 parts by weight prepares graphene oxide using Hummers method is improved, in preparation process, graphite and
Concentrated sulfuric acid mass ratio is 10:100, and graphene oxide/concentrated sulfuric acid dispersion liquid is obtained after fully reacting；
(2) it takes the sucrose of 20 parts by weight and the water of 1.5 parts by weight to be uniformly mixed, is added to the oxidation stone that step (1) obtains
In black alkene/concentrated sulfuric acid dispersion liquid, it is stirred continuously, obtains viscous pastes；
(3) viscous pastes that step (2) obtains 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 kept the temperature, porous graphene/active carbon compound adsorbent is obtained.
Through above step, obtained porous graphene/active carbon compound adsorbent is black foam shape, density 0.51g/
cm3, specific surface area 1420m2/ g, pore volume 1.1cm3/ g, methylenum careuleum adsorptive value are 334ml/g.
Embodiment 5:
(1) graphite for taking 10 parts by weight prepares graphene oxide using Hummers method is improved, in preparation process, graphite and
Concentrated sulfuric acid mass ratio is 10:100, and graphene oxide/concentrated sulfuric acid dispersion liquid is obtained after fully reacting；
(2) it takes the sucrose of 30 parts by weight and the water of 4 parts by weight to be uniformly mixed, is added to the graphite oxide that step (1) obtains
In alkene/concentrated sulfuric acid dispersion liquid, it is stirred continuously, obtains viscous pastes；
(3) viscous pastes that step (2) obtains 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 kept the temperature, porous graphene/active carbon compound adsorbent is obtained.
Through above step, obtained porous graphene/active carbon compound adsorbent is black foam shape, density 0.68g/
cm3, specific surface area 1150m2/ g, pore volume 0.73cm3/ g, methylenum careuleum adsorptive value are 309ml/g.
Embodiment 6:
(1) graphite for taking 30 parts by weight prepares graphene oxide using Hummers method is improved, in preparation process, graphite and
Concentrated sulfuric acid mass ratio is 10:100, and graphene oxide/concentrated sulfuric acid dispersion liquid is obtained after fully reacting；
(2) it takes the carbohydrate powder of 40 parts by weight to be uniformly mixed with the water of 5 parts by weight, is added to the oxidation that step (1) obtains
In graphene/concentrated sulfuric acid dispersion liquid, it is stirred continuously, obtains viscous pastes；
(3) viscous pastes that step (2) obtains 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 kept the temperature, porous graphene/active carbon compound adsorbent is obtained.
Through above step, obtained porous graphene/active carbon compound adsorbent is black foam shape, density 0.79g/
cm3, specific surface area 520m2/ g, pore volume 0.33cm3/ g, methylenum careuleum adsorptive value are 265ml/g.
Embodiment 7:
(1) graphite for taking 10 parts by weight prepares graphene oxide using Hummers method is improved, in preparation process, graphite and
Concentrated sulfuric acid mass ratio is 10:100, and graphene oxide/concentrated sulfuric acid dispersion liquid is obtained after fully reacting；
(2) it takes the starch of 20 parts by weight and the water of 4 parts by weight to be uniformly mixed, is added to the graphite oxide that step (1) obtains
In alkene/concentrated sulfuric acid dispersion liquid, it is stirred continuously, obtains viscous pastes；
(3) viscous pastes that step (2) obtains 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 kept the temperature, porous graphene/active carbon compound adsorbent is obtained.
Through above step, obtained porous graphene/active carbon compound adsorbent is black foam shape, density 0.58g/
cm3, specific surface area 1370m2/ g, pore volume 0.88cm3/ g, methylenum careuleum adsorptive value are 341ml/g.
Claims (3)
1. a kind of preparation method of porous graphene/active carbon compound adsorbent, which comprises the following steps:
(1) graphite for taking 10 ~ 30 parts by weight prepares graphene oxide using Hummers method is improved, in preparation process, graphite and
Concentrated sulfuric acid mass ratio is 10 ~ 30:100, and graphene oxide/concentrated sulfuric acid dispersion liquid is obtained after fully reacting；
(2) it takes the carbohydrate powder of 10 ~ 40 parts by weight to be uniformly mixed with the water of 1 ~ 5 parts by weight, is added to the oxidation that step (1) obtains
In graphene/concentrated sulfuric acid dispersion liquid, it is stirred continuously, obtains viscous pastes；
(3) viscous pastes that step (2) obtains 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 heat preservation or so obtains porous graphene/active carbon compound adsorbent.
2. porous graphene/active carbon compound adsorbent that a kind of claim 1 is prepared, which is characterized in that by active carbon
It is formed with graphene, density is 0.2 ~ 0.8g/cm3Left and right, specific surface area are 500 ~ 2000 m2/ g, pore volume is about 0.3 ~
2cm3/g。
3. the method according to claim 1, wherein carbohydrate powder described in step (2) be xylose, sucrose,
One of glucose, fructose, lactose, starch, cellulose etc. are a variety of.
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| 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 |
| CN109192992B (en) * | 2018-08-24 | 2021-07-02 | 东华大学 | Pd/MGF composite material and preparation and application thereof |
| 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 |
| CN110844902B (en) * | 2019-11-20 | 2023-05-26 | 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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