CN109399615A - A kind of preparation method of the using biomass resource 3D- grapheme material as carbon source - Google Patents
A kind of preparation method of the using biomass resource 3D- grapheme material as carbon source Download PDFInfo
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- CN109399615A CN109399615A CN201811423554.7A CN201811423554A CN109399615A CN 109399615 A CN109399615 A CN 109399615A CN 201811423554 A CN201811423554 A CN 201811423554A CN 109399615 A CN109399615 A CN 109399615A
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/20—Controlling water pollution; Waste water treatment
- Y02A20/208—Off-grid powered water treatment
- Y02A20/212—Solar-powered wastewater sewage treatment, e.g. spray evaporation
Abstract
The present invention relates to a kind of preparation methods of 3D- grapheme material as carbon source of using biomass resource, steps are as follows: (1) in aqueous solution by biomass dissolution, after stirring to dissolve, water-soluble inorganic salt is added, continue stirring and form uniform solution to it, aforesaid liquid is titrated in organic solvent, white solid is obtained, it is dried in a vacuum drying oven to get the mixture of biomass and salt is arrived；(2) object is put into tube furnace and is carbonized, and in water by the sample dispersion after carbonization, filtering obtains black solid to get 3D- grapheme material.3D grapheme material good water solubility made from the method for the present invention, large specific surface area, conductivity are high, sheet of material thickness is uniform, about 1~2nm, there is stronger absorption property to pollutant in waste water from dyestuff, there is stronger absorption property to organic dyestuff crystal violet or methylenum careuleum, there is preferable absorbability near infrared light and thermal energy can be converted it into.
Description
Technical field
The invention belongs to functionalization technical field of material, especially a kind of 3D- for using biomass resource as carbon source
The preparation method of grapheme material.
Background technique
Graphene is that one kind by sp2 hydridization carbon constitutes cellular 2D plane carbon material, because of it with good physics or
Chemical property is widely used in battery, water body if conductivity is high, flexibility is good, large specific surface area and near infrared light thermal transition
The fields such as purification.3D graphene refers to that graphene film interlayer is interconnected to tridimensional network, and this three-dimensional structure solves single
A large amount of multilayer subchannel is produced again while stacking between piece graphene, is very beneficial for mass transfer, absorption and load.
Currently, the method for preparing 3D graphene is varied, including the chemical vapor deposition using metal foam as template
Method (CVD) and 3D structure is self-assembled by graphene oxide (GO).But these methods are complicated for operation, cost of manufacture is high.Closely
Nian Laiyong biomass prepares graphene as a member new in graphene preparation as carbon source, but there are no phases currently on the market
The product of pass is the graphene that three-dimensional structure is prepared using biomass as carbon source, thus make it is a kind of use biomass resource as
The 3D- graphene of carbon source is very important.
By retrieval, patent publication us relevant to present patent application is not yet found.
Summary of the invention
Present invention aims in place of the deficiencies in the prior art, a kind of 3D- stone for using biomass resource as carbon source is provided
The preparation method of black alkene material, this method good biocompatibility, method are simple, and 3D- grapheme material obtained is with higher
Conductivity, near infrared light with good absorption and to crystal violet and methylene blue dye with good adsorptivity.
The technical solution adopted by the present invention to solve the technical problems is:
A kind of preparation method of the using biomass resource 3D- grapheme material as carbon source, steps are as follows:
(1) in aqueous solution by biomass dissolution, after stirring to dissolve, water-soluble inorganic salt is added, continues to stir to it
Uniform solution is formed, aforesaid liquid is titrated in organic solvent, white solid is obtained, dries in a vacuum drying oven, i.e.,
Obtain the mixture of biomass and salt；
Wherein, the biomass: the mass ratio of salt is 1:1~1:10；
By step (1) in the mixture of biomass and salt be put into tube furnace and be carbonized, by the sample dispersion after carbonization in water
In, filtering obtains black solid to get 3D- grapheme material.
Moreover, (1) middle biomass is water-soluble biological molecule to the step.
Moreover, the water-soluble biological molecule is amino acid or sugar.
Moreover, the step (1) in whipping temp be room temperature, 20~30 DEG C.
Moreover, (1) middle water-soluble inorganic salt is copper sulphate or sodium sulphate or potassium chloride or sodium chloride to the step.
Moreover, (1) middle organic solvent is organic solvent miscible with water to the step.
Moreover, the organic solvent miscible with water is ethyl alcohol or isopropanol or methanol.
Moreover, the step (1) in titration when be titrated in organic solvent with syringe pump, and syringe pump rate of titration is
200-1000ul/min。
Moreover, (1) middle dry actual conditions are 80~120 DEG C, 4~12 hours to the step.
Moreover, the step (2) in when being carbonized in tube furnace, the temperature program of tube furnace are as follows:
200~500 DEG C are raised to from room temperature with 1~5 DEG C/min and is maintained 1~2 hour, then are warming up to 1~5 DEG C/min
It 500~900 DEG C, maintains 1~2 hour.
The advantages of present invention obtains and good effect are as follows:
1,3D grapheme material good water solubility made from the method for the present invention, large specific surface area, conductivity are high, material piece thickness
Uniformly, about 1~2nm has stronger absorption property to pollutant in waste water from dyestuff, to organic dyestuff crystal violet or methylene to degree
Indigo plant has stronger absorption property, has preferable absorbability near infrared light and can convert it into thermal energy；Furthermore this method
It selects biomass as carbon source, can be mass produced and cost is relatively low, greatly save production cost, there is wide answer
Use prospect.
2, the method for the present invention synthesis process is simple, and good biocompatibility, condition is easily controllable, obtained material structure compared with
It is uniform, there is preferable conductivity, near infrared light thermal transition, water-soluble and specific surface area is used as battery electrode material
Material, heating film, adsorbent realize a kind of material multiple use, have broad application prospects.
3, the synthesis process of 3D graphene made from the method for the present invention is simple, and the removal process of subsequent template salt operates letter
It is single, it need to only be dissolved with water, and this water-soluble inorganic salt secondary can recycle, there is very wide application prospect.
4, the formation of the 3D structure of the 3D graphene of the method for the present invention only needs single step reaction can be obtained, reaction process letter
It is single, it improves work efficiency.
5, the carbon source of the 3D graphene of the method for the present invention selects biomass, such as amino acid, and sugar has greatly been saved and has been produced into
This, has broad application prospects.
Detailed description of the invention
Fig. 1 is that the present invention uses biomass sources as the scanning electron microscope (SEM) photograph of 3D- grapheme material made from carbon source, from Fig. 1
It can be seen that lamellar spacing made from the method for the present invention is uniform, each interlayer is interconnected to 3D structure；
Fig. 2 is that the present invention uses biomass sources as the transmission electron microscope picture of 3D- grapheme material made from carbon source, from Fig. 2
It can be seen that material piece made from the method for the present invention at very thin, lamellar spacing 1-2nm；
Fig. 3 is that the present invention uses biomass sources as the XRD diagram of 3D- grapheme material made from carbon source, can from Fig. 3
The crystal form of material made from the method for the present invention is fine out.
Specific embodiment
The embodiment of the present invention is described in detail below, it should be noted that the present embodiment is narrative, is not limited
, this does not limit the scope of protection of the present invention.
Raw material used in the present invention is unless otherwise specified conventional commercial product；Used in the present invention
Method is unless otherwise specified the conventional method of this field.
Embodiment 1
It is a kind of with the preparation method for the 3D- grapheme material that protein is carbon source, steps are as follows:
(1) in aqueous solution by bovine serum albumin dissolution, after 20 DEG C stir to dissolve, sodium sulphate is added, continues stirring extremely
It forms uniform solution, and aforesaid liquid is titrated in ethyl alcohol (rate of titration 200ul/min) with syringe pump, and it is solid to obtain white
Body dries 4~12 hours in 80 DEG C~120 DEG C of vacuum oven to get the mixture for arriving bovine serum albumin and salt；
Wherein, the mass ratio of the bovine serum albumin and salt is 1:3；
(2) by step, (1) the mixture of protein and salt is put into tube furnace and is carbonized, by the sample dispersion after carbonization in water
In, filtering obtains black solid to get 3D- grapheme material.
Wherein temperature program are as follows: be raised to 300 DEG C from room temperature with 2 DEG C/min and maintain 2 hours, then with 3 DEG C/min heating
To 500 DEG C, maintain 1 hour.
Embodiment 2
It is a kind of with the preparation method for the 3D- grapheme material that glycine is carbon source, steps are as follows:
(1) in aqueous solution by glycine dissolution, after 20 DEG C stir to dissolve, potassium chloride is added, continues stirring to its shape
At uniform solution, aforesaid liquid is titrated in isopropanol (rate of titration 300ul/min) with syringe pump, it is solid to obtain white
Body dries 4~12 hours in 80 DEG C~120 DEG C of vacuum oven to get the mixture for arriving glycine and salt；
Wherein, the mass ratio of the glycine and salt is 1:5；
(2) by step, (1) the mixture of glycine and salt is put into tube furnace and is carbonized, by the sample dispersion after carbonization in water
In, filtering obtains black solid to get 3D- grapheme material.
Wherein temperature program are as follows: be raised to 200 DEG C from room temperature with 3 DEG C/min and maintain 1~2 hour, then with 1 DEG C/min liter
Temperature maintains 1~2 hour to 600 DEG C.
Embodiment 3
It is a kind of with the preparation method for the 3D- grapheme material that glutamic acid is carbon source, steps are as follows:
(1) in aqueous solution by glutamic acid dissolution, after room temperature (25 DEG C) stirs to dissolve, copper sulphate is added, continues to stir
Uniform solution is formed to it, aforesaid liquid is titrated in isopropanol (rate of titration 500ul/min) with syringe pump, is obtained white
Color solid dries 4~12 hours in 80 DEG C~120 DEG C of vacuum oven to get the mixture for arriving glutamic acid and salt；
Wherein, the mass ratio of the glutamic acid and salt is 1:8；
(2) by step, (1) the mixture of glutamic acid and salt is put into tube furnace and is carbonized, by the sample dispersion after carbonization in water
In, filtering obtains black solid to get 3D- grapheme material.
Wherein temperature program are as follows: be raised to 350 DEG C from room temperature with 2 DEG C/min and maintain 1~2 hour, then with 3 DEG C/min liter
Temperature maintains 1~2 hour to 700 DEG C.
Embodiment 4
A kind of preparation method for using the sugared 3D- grapheme material as carbon source, steps are as follows:
(1) in deionized water by glucose dissolution, after stirring at normal temperature makes it dissolve, sodium chloride, stirring to its formation are added
Aforesaid liquid is titrated in ethyl alcohol (rate of titration 300ul/min) with syringe pump, obtains white solid by uniform solution, in
4~12 hours are dried in 80 DEG C~120 DEG C of vacuum oven to get the mixture for arriving glucose and sodium chloride；
Wherein, the mass ratio of the glucose and salt is 1:5；
(2) by step, (1) the mixture of glucose and salt is put into tube furnace and is carbonized, by the sample dispersion after carbonization in water
In, filtering obtains black solid to get 3D- grapheme material.
Wherein temperature program are as follows: be raised to 300 DEG C from room temperature with 5 DEG C/min and maintain 1~2 hour, then with 3 DEG C/min liter
Temperature maintains 1~2 hour to 600 DEG C.
Embodiment 5
A kind of preparation method for using the sugared 3D- grapheme material as carbon source, steps are as follows:
(1) in deionized water by glucose dissolution, after stirring at normal temperature makes it dissolve, sodium chloride, stirring to its formation are added
Aforesaid liquid is titrated in methanol (rate of titration 600ul/min) by uniform solution with syringe pump, and it is solid that centrifugation obtains white
Body is dried in a vacuum drying oven to get the mixture of glucose and sodium chloride is arrived；
Wherein, the mass ratio of the glucose and sodium chloride is 1:6；
(2) by step, (1) glucose and potassium chloride mixture are put into tube furnace and are carbonized, by the sample dispersion after carbonization in water
In, filtering obtains black solid to get 3D- grapheme material.
Wherein temperature program are as follows: be raised to 500 DEG C from room temperature with 3 DEG C/min and maintain 1~2 hour, then with 5 DEG C/min liter
Temperature maintains 1~2 hour to 900 DEG C.
The present invention uses biomass sources as the coherent detection of the 3D- grapheme material of carbon source:
1, the scanning electron microscope (SEM) photograph that the present invention uses biomass sources as the 3D- grapheme material of carbon source is tested, as a result such as Fig. 1 institute
Show, lamellar spacing of the present invention is uniform as can be seen from Figure 1, and each interlayer is interconnected to 3D structure；
2, the transmission electron microscope picture that the present invention uses biomass sources as the 3D- grapheme material of carbon source detects, as a result such as Fig. 2 institute
Show, the lamella of material of the present invention is very thin as can be seen from Figure 2, lamellar spacing 1-2nm；
3, the present invention uses biomass sources as the XRD diagram of the 3D- grapheme material of carbon source, as a result as shown in figure 3, from Fig. 3
In can be seen that the crystal form of material of the present invention is fine.
Although disclosing the embodiment of the present invention for the purpose of illustration, it will be appreciated by those skilled in the art that: not
Be detached from the present invention and spirit and scope of the appended claims in, various substitutions, changes and modifications be all it is possible, therefore, this
The range of invention is not limited to the embodiment and attached drawing disclosure of that.
Claims (10)
1. a kind of preparation method for the 3D- grapheme material as carbon source of using biomass resource, it is characterised in that: steps are as follows:
(1) in aqueous solution by biomass dissolution, after stirring to dissolve, water-soluble inorganic salt is added, continues stirring to its formation
Uniform solution, aforesaid liquid is titrated in organic solvent, obtains white solid, is dried in a vacuum drying oven to get arriving
The mixture of biomass and salt；
Wherein, the biomass: the mass ratio of salt is 1:1~1:10；
By step (1) in the mixture of biomass and salt be put into tube furnace and be carbonized, in water by the sample dispersion after carbonization,
Filtering, obtains black solid to get 3D- grapheme material.
2. the preparation method of 3D- grapheme material as carbon source according to claim 1 of using biomass resource, feature
Be: (1) middle biomass is water-soluble biological molecule to the step.
3. the preparation method of 3D- grapheme material as carbon source according to claim 2 of using biomass resource, feature
Be: the water-soluble biological molecule is amino acid or sugar.
4. the preparation method of 3D- grapheme material as carbon source according to claim 1 of using biomass resource, feature
Be: the step (1) in whipping temp be room temperature, 20~30 DEG C.
5. the preparation method of 3D- grapheme material as carbon source according to claim 1 of using biomass resource, feature
Be: (1) middle water-soluble inorganic salt is copper sulphate or sodium sulphate or potassium chloride or sodium chloride to the step.
6. the preparation method of 3D- grapheme material as carbon source according to claim 1 of using biomass resource, feature
Be: (1) middle organic solvent is organic solvent miscible with water to the step.
7. the preparation method of 3D- grapheme material as carbon source according to claim 6 of using biomass resource, feature
Be: the organic solvent miscible with water is ethyl alcohol or isopropanol or methanol.
8. the preparation method of 3D- grapheme material as carbon source according to claim 1 of using biomass resource, feature
Be: the step (1) in titration when be titrated in organic solvent with syringe pump, and syringe pump rate of titration be 200-1000
ul/min。
9. the preparation method of 3D- grapheme material as carbon source according to claim 1 of using biomass resource, feature
Be: (1) middle dry actual conditions are 80~120 DEG C, 4~12 hours to the step.
10. the preparation of 3D- grapheme material as carbon source according to any one of claims 1 to 9 of using biomass resource
Method, it is characterised in that: the step (2) in when being carbonized in tube furnace, the temperature program of tube furnace are as follows:
200~500 DEG C are raised to from room temperature with 1~5 DEG C/min and is maintained 1~2 hour, then are warming up to 500 with 1~5 DEG C/min
It~900 DEG C, maintains 1~2 hour.
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Cited By (2)
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| CN111547709A (en) * | 2020-05-09 | 2020-08-18 | 九江学院 | Biomass three-dimensional porous graphene and preparation method thereof |
| WO2024006663A3 (en) * | 2022-06-24 | 2024-02-29 | University Of Virginia Patent Foundation | Graphene and methods of making graphene |
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