CN109437168A - A kind of graphene hydrogel and preparation method thereof - Google Patents
A kind of graphene hydrogel and preparation method thereof Download PDFInfo
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- CN109437168A CN109437168A CN201910004249.2A CN201910004249A CN109437168A CN 109437168 A CN109437168 A CN 109437168A CN 201910004249 A CN201910004249 A CN 201910004249A CN 109437168 A CN109437168 A CN 109437168A
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- graphene hydrogel
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- hydrogel
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
Abstract
The present invention provides a kind of preparation methods of graphene hydrogel, comprising the following steps: after a) diluting the alkali leaching liquor of coal, carries out pH adjusting, then through ultrasonic disperse, obtain raw material mixed liquor；B) the raw material mixed liquor for obtaining step a) carries out hydro-thermal reaction, then successively obtains graphene hydrogel through cooling, washing, drying.Compared with prior art, preparation method provided by the invention, using specific process step and condition, realizes preferable interaction using the alkali leaching liquor of coal as raw material, the graphene hydrogel with unique three-dimensional hole macroscopic view three-dimensional-structure is prepared, realizing turns waste into wealth；And the 3 D stereo reticular structure stability for the graphene hydrogel being prepared is good, the specific surface area with superelevation can be applied to the numerous areas such as lithium ion battery negative material, adsorbent material and catalyst carrier.
Description
Technical field
The present invention relates to carbon material technical fields more particularly to a kind of graphene hydrogel and preparation method thereof.
Background technique
In recent years, graphene is as a kind of emerging carbon material by the concern of domestic and international researcher.Graphene has
Many excellent properties, such as optics, electricity, mechanical characteristic, to be widely used in energy storage, catalysis, sensor and suction
Attached field.The theoretical specific surface area of two-dimensional graphene material is 2630m2/ g, since the Van der Waals force of graphene film interlayer causes
Agglomeration so that its actual specific surface area is well below theoretical value.Grapheme material is prepared into three-dimensional netted
The three-dimensional macrostructure of crosslinking can solve this defect to a certain extent.Such as application No. is 201410563543.4 China
Patent discloses a kind of Anti-pressure graphene hydrogel and preparation method thereof, uses graphene oxide for presoma, adulterates high electricity
The phytic acid of conductance is prepared into three-dimensional grapheme hydrogel through hydro-thermal reaction.For another example application No. is the China of 201210330721.X
Patent discloses a kind of preparation method of nitrogen-doped graphene hydrogel, and organic amine is added dropwise in graphene oxide water solution and passes through
Hydrothermal synthesis reaction obtains nitrogen-doped graphene hydrogel.
But the preparation method of graphene hydrogel in the prior art is higher to ingredient requirement, preparation process is complicated；And
And the 3 D stereo reticular structure stability for the graphene hydrogel being prepared is not high, limit its specific surface area into one
Step improves.
Summary of the invention
In view of this, the present invention provides the purpose of the present invention is to provide a kind of graphene hydrogel and preparation method thereof
Preparation method using the alkali leaching liquor of coal as raw material, the graphene with unique three-dimensional hole macroscopic view three-dimensional-structure has been prepared
Hydrogel, realizing turns waste into wealth；And the graphene hydrogel being prepared has the specific surface area of superelevation.
The present invention provides a kind of preparation methods of graphene hydrogel, comprising the following steps:
A) after diluting the alkali leaching liquor of coal, pH adjusting is carried out, then through ultrasonic disperse, obtain raw material mixed liquor；
B) the raw material mixed liquor for obtaining step a) carries out hydro-thermal reaction, then successively obtains stone through cooling, washing, drying
Black alkene hydrogel.
Preferably, the alkali leaching liquor of coal described in step a) includes the organic matter that content is 1wt%~20wt%.
Preferably, diluted process described in step a) specifically:
The alkali leaching liquor and deionized water for taking coal are according to mass ratio (0.5~10): 1 is diluted, the alkali after being diluted
Leachate.
Preferably, regulator used in the process that pH described in step a) is adjusted includes inorganic acid and/or organic acid.
Preferably, the pH value that pH described in step a) is adjusted is 5~7.5.
Preferably, the power of ultrasonic disperse described in step a) is 50W~300W, and the time is 10min~90min.
Preferably, the temperature of hydro-thermal reaction described in step a) is 90 DEG C~180 DEG C, and the time is 6h~for 24 hours.
Preferably, temperature cooling described in step a) is 20 DEG C~30 DEG C.
The present invention also provides a kind of graphene hydrogel, the preparation method as described in above-mentioned technical proposal is made.
The present invention provides a kind of preparation methods of graphene hydrogel, comprising the following steps: a) by the alkali leaching liquor of coal
After dilution, pH adjusting is carried out, then through ultrasonic disperse, obtain raw material mixed liquor；B) the raw material mixed liquor for obtaining step a) carries out
Hydro-thermal reaction, then successively graphene hydrogel is obtained through cooling, washing, drying.Compared with prior art, provided by the invention
Preparation method, using specific process step and condition, realizes preferable interaction using the alkali leaching liquor of coal as raw material, preparation
The graphene hydrogel with unique three-dimensional hole macroscopic view three-dimensional-structure is obtained, realizing turns waste into wealth；And be prepared
The 3 D stereo reticular structure stability of graphene hydrogel is good, and the specific surface area with superelevation can be applied to lithium ion battery
The numerous areas such as negative electrode material, adsorbent material and catalyst carrier.
In addition, preparation method raw material provided by the invention is easy to get, is at low cost, and simple process, high yield rate, and realize
The resource utilization of waste liquid, it is environmentally protective, it has broad application prospects.
Detailed description of the invention
Fig. 1 is the exterior appearance schematic diagram for the graphene hydrogel that the embodiment of the present invention 1~5 provides；
Fig. 2 is the scanning electron microscope (SEM) photograph for the graphene hydrogel that the embodiment of the present invention 1 provides；
Fig. 3 is the scanning electron microscope (SEM) photograph for the graphene hydrogel that the embodiment of the present invention 2 provides；
Fig. 4 is the scanning electron microscope (SEM) photograph for the graphene hydrogel that the embodiment of the present invention 3 provides；
Fig. 5 is the scanning electron microscope (SEM) photograph for the graphene hydrogel that the embodiment of the present invention 4 provides；
Fig. 6 is the scanning electron microscope (SEM) photograph for the graphene hydrogel that the embodiment of the present invention 5 provides.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
The present invention provides a kind of preparation methods of graphene hydrogel, comprising the following steps:
A) after diluting the alkali leaching liquor of coal, pH adjusting is carried out, then through ultrasonic disperse, obtain raw material mixed liquor；
B) the raw material mixed liquor for obtaining step a) carries out hydro-thermal reaction, then successively obtains stone through cooling, washing, drying
Black alkene hydrogel.
After the present invention first dilutes the alkali leaching liquor of coal, pH adjusting is carried out, then through ultrasonic disperse, obtain raw material mixing
Liquid.In the present invention, the alkali leaching liquor of the coal preferably includes the organic matter that content is 1wt%~20wt%, more preferably
3wt%~8wt%；It is also preferable to include the NaOH that content is 5wt%~20wt% for the alkali leaching liquor of the coal, more preferably
8wt%~12wt%.In invention, the main component of the organic matter is alkali lignin.
The present invention is not particularly limited the source of the leachate of the coal, using coal well known to those skilled in the art
The alkaline waste liquor generated during chemical deliming；Contain organic matter in the alkaline waste liquor, with the progress of reaction, organic matter
It will constantly accumulate, eventually having an impact to reaction.Applicants have found that being dissolved in having in above-mentioned alkaline waste liquor
Machine molecule has three-dimensional space network structure, with being cross-linked into it by self assembly with 3 D stereo reticular structure graphene
The possibility of hydrogel macroscopic body.In the preferred embodiment of the invention, the leachate of the coal is that chemical method prepares ultra-clean coal
The alkali leaching liquor generated in the process.
In the present invention, the diluted process is preferred specifically:
The alkali leaching liquor and deionized water for taking coal are according to mass ratio (0.5~10): 1 is diluted, the alkali after being diluted
Leachate；
More preferably:
The alkali leaching liquor and deionized water for taking coal are according to mass ratio (3~5): 1 is diluted, and the alkali after being diluted leaches
Liquid.
After alkali leaching liquor after obtaining the dilution, the alkali leaching liquor after obtained dilution is carried out pH adjusting by the present invention,
Again through ultrasonic disperse, raw material mixed liquor is obtained.In the present invention, regulator used in the process that the pH is adjusted preferably includes nothing
Machine acid and/or organic acid, more preferably organic acid.In the preferred embodiment of the invention, the regulator is ascorbic acid.This
Invention is not particularly limited the source of the regulator, using commercial goods well known to those skilled in the art or laboratory from
Product.
In the present invention, the pH value that the pH is adjusted is preferably 5~7.5, and more preferably 5.5~6.5.
In the present invention, the frequency of the ultrasonic disperse is preferably 50W~300W, more preferably 100W~200W；It is described
The time of ultrasonic disperse is preferably 10min~90min, more preferably 30min~60min.
After obtaining the raw material mixed liquor, obtained raw material mixed liquor is carried out hydro-thermal reaction by the present invention, then successively through cold
But, wash, is dry, obtaining graphene hydrogel.The present invention is not particularly limited the container of the hydro-thermal reaction, using ability
The stainless steel cauldron of polytetrafluoroethylsubstrate substrate is had known to field technique personnel.
In the present invention, the temperature of the hydro-thermal reaction is preferably 90 DEG C~180 DEG C, and more preferably 150 DEG C~170 DEG C,
Most preferably 160 DEG C；The time of the hydro-thermal reaction is preferably 6h~for 24 hours, more preferably 6h~18h.
The present invention is by above-mentioned hydro-thermal reaction, and the alkali leaching liquor of the coal under handling specific process step and condition is in hydro-thermal
Self assembly is carried out under environment, is cross-linked into 3 D stereo reticular structure graphene hydrogel macroscopic body.
In the present invention, the temperature of the cooling is preferably 20 DEG C~30 DEG C, more preferably 25 DEG C.The present invention is washed to described
The mode washed is not particularly limited, the technical solution washed using deionized water well known to those skilled in the art.This hair
The bright mode to the drying is not particularly limited, i.e. using the technical solution dried under room temperature well known to those skilled in the art
It can.
Preparation method provided by the invention, using specific process step and condition, is realized using the alkali leaching liquor of coal as raw material
Preferable interaction, has been prepared the graphene hydrogel with unique three-dimensional hole macroscopic view three-dimensional-structure, has realized
Turn waste into wealth；And the 3 D stereo reticular structure stability for the graphene hydrogel being prepared is good, the specific surface with superelevation
Product, can be applied to the numerous areas such as lithium ion battery negative material, adsorbent material and catalyst carrier.In addition, the present invention provides
Preparation method raw material be easy to get, be at low cost, simple process, high yield rate, and realize the resource utilization of waste liquid, green ring
It protects, has broad application prospects.
The present invention also provides a kind of graphene hydrogel, the preparation method as described in above-mentioned technical proposal is made.This hair
The graphene hydrogel of bright offer is graphene oxide hydrogel, has good three-dimensional pore space macroscopic view three-dimensional-structure and macroscopic view knot
The specific surface area of structure stability and superelevation has great application prospect in energy storage, catalysis, adsorbing domain.
The present invention provides a kind of preparation methods of graphene hydrogel, comprising the following steps: a) by the alkali leaching liquor of coal
After dilution, pH adjusting is carried out, then through ultrasonic disperse, obtain raw material mixed liquor；B) the raw material mixed liquor for obtaining step a) carries out
Hydro-thermal reaction, then successively graphene hydrogel is obtained through cooling, washing, drying.Compared with prior art, provided by the invention
Preparation method, using specific process step and condition, realizes preferable interaction using the alkali leaching liquor of coal as raw material, preparation
The graphene hydrogel with unique three-dimensional hole macroscopic view three-dimensional-structure is obtained, realizing turns waste into wealth；And be prepared
The 3 D stereo reticular structure stability of graphene hydrogel is good, and the specific surface area with superelevation can be applied to lithium ion battery
The numerous areas such as negative electrode material, adsorbent material and catalyst carrier.
In addition, preparation method raw material provided by the invention is easy to get, is at low cost, and simple process, high yield rate, and realize
The resource utilization of waste liquid, it is environmentally protective, it has broad application prospects.
In order to further illustrate the present invention, technical solution provided by the invention is retouched in detail below with reference to embodiment
It states.The alkali leaching liquor of coal used in following embodiment of the present invention is that chemical method prepares the alkali leaching generated during ultra-clean coal
Liquid, alkali (NaOH) concentration be 8wt%~12wt%, the content of organic matter be 3wt%~8wt%, the organic matter it is main at
It is divided into alkali lignin.
Embodiment 1
(1) alkali leaching liquor and deionized water for taking coal are diluted according to mass ratio 4:1, and the alkali after being diluted leaches
Liquid；Then Vitamin C acid for adjusting pH value is added, until pH value is 6, then carries out ultrasonic disperse 30min at 200W, it is mixed to obtain raw material
Close liquid.
(2) the raw material mixed liquor that step (1) obtains is transferred in hydrothermal reaction kettle, hydro-thermal reaction is carried out at 160 DEG C
12h；After reaction, it is cooled to room temperature, is dried at 25 DEG C after washing, obtain graphene hydrogel.
The exterior appearance schematic diagram for the graphene hydrogel that the embodiment of the present invention 1 provides is referring to shown in (a) in Fig. 1；This hair
The scanning electron microscope (SEM) photograph for the graphene hydrogel that bright embodiment 1 provides is shown in Figure 2.By Fig. 1~2 it is found that the embodiment of the present invention 1
The 3 D stereo reticular structure stability of the graphene hydrogel of offer is high, forms unique three-dimensional hole macroscopic view three-dimensional-structure；And
And through detecting, the specific surface area for the graphene hydrogel that the embodiment of the present invention 1 provides is 962m2/ g, the specific surface with superelevation
Product, is conducive to it in the application of the numerous areas such as lithium ion battery negative material, adsorbent material and catalyst carrier.
Embodiment 2
The preparation method provided using embodiment 1, difference are: the alkali leaching liquor of coal is pressed with deionized water in step (1)
It is diluted according to mass ratio 3:1；Obtain graphene hydrogel.
Through detecting, the 3 D stereo reticular structure stability for the graphene hydrogel that the embodiment of the present invention 2 provides is high, is formed
Unique three-dimensional hole macroscopic view three-dimensional-structure, in Fig. 1 shown in (b) and Fig. 3；And its specific surface area is 838m2/ g has superelevation
Specific surface area.
Embodiment 3
The preparation method provided using embodiment 1, difference are: the alkali leaching liquor of coal is pressed with deionized water in step (1)
It is diluted according to mass ratio 5:1；Obtain graphene hydrogel.
Through detecting, the 3 D stereo reticular structure stability for the graphene hydrogel that the embodiment of the present invention 3 provides is high, is formed
Unique three-dimensional hole macroscopic view three-dimensional-structure, in Fig. 1 shown in (c) and Fig. 4；And its specific surface area is 754m2/ g has superelevation
Specific surface area.
Embodiment 4
The preparation method provided using embodiment 1, difference are: the time of hydro-thermal reaction described in step (2) is 6h；?
To graphene hydrogel.
Through detecting, the 3 D stereo reticular structure stability for the graphene hydrogel that the embodiment of the present invention 4 provides is high, is formed
Unique three-dimensional hole macroscopic view three-dimensional-structure, in Fig. 1 shown in (d) and Fig. 5；And its specific surface area is 890m2/ g has superelevation
Specific surface area.
Embodiment 5
The preparation method provided using embodiment 1, difference are: the time of hydro-thermal reaction described in step (2) is 18h；
Obtain graphene hydrogel.
Through detecting, the 3 D stereo reticular structure stability for the graphene hydrogel that the embodiment of the present invention 5 provides is high, is formed
Unique three-dimensional hole macroscopic view three-dimensional-structure, in Fig. 1 shown in (e) and Fig. 6；And its specific surface area is 772m2/ g has superelevation
Specific surface area.
The above description of the disclosed embodiments, enables those skilled in the art to implement or use the present invention.It is right
A variety of modifications of these embodiments will be readily apparent to those skilled in the art, and as defined herein one
As principle can realize in other embodiments without departing from the spirit or scope of the present invention.Therefore, the present invention will
It will not be intended to be limited to the embodiments shown herein, and be to fit to consistent with the principles and novel features disclosed herein
Widest scope.
Claims (9)
1. a kind of preparation method of graphene hydrogel, comprising the following steps:
A) after diluting the alkali leaching liquor of coal, pH adjusting is carried out, then through ultrasonic disperse, obtain raw material mixed liquor；
B) the raw material mixed liquor for obtaining step a) carries out hydro-thermal reaction, then successively obtains graphene through cooling, washing, drying
Hydrogel.
2. preparation method according to claim 1, which is characterized in that the alkali leaching liquor of coal described in step a) includes content
For the organic matter of 1wt%~20wt%.
3. preparation method according to claim 1, which is characterized in that diluted process described in step a) specifically:
The alkali leaching liquor and deionized water for taking coal are according to mass ratio (0.5~10): 1 is diluted, and the alkali after being diluted leaches
Liquid.
4. preparation method according to claim 1, which is characterized in that tune used in the process that pH described in step a) is adjusted
Saving agent includes inorganic acid and/or organic acid.
5. preparation method according to claim 1, which is characterized in that pH described in step a) adjust pH value be 5~
7.5。
6. preparation method according to claim 1, which is characterized in that the power of ultrasonic disperse described in step a) is 50W
~300W, time are 10min~90min.
7. preparation method according to claim 1, which is characterized in that the temperature of hydro-thermal reaction described in step a) is 90 DEG C
~180 DEG C, the time is 6h~for 24 hours.
8. preparation method according to claim 1, which is characterized in that cooling temperature described in step a) is 20 DEG C~30
℃。
9. a kind of graphene hydrogel, which is characterized in that be made by preparation method according to any one of claims 1 to 8.
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| CN103466613A (en) * | 2013-10-11 | 2013-12-25 | 中南林业科技大学 | Method for preparing graphene from lignin |
| CN105217607A (en) * | 2015-08-22 | 2016-01-06 | 苏州正业昌智能科技有限公司 | A kind of graphene preparation method based on xylogen |
| CN105439135A (en) * | 2015-12-30 | 2016-03-30 | 成都新柯力化工科技有限公司 | Method for preparing graphene from lignin |
| CN106241780A (en) * | 2016-07-19 | 2016-12-21 | 华南理工大学 | A kind of method preparing Graphene for raw material with lignin |
| US20170113936A1 (en) * | 2013-06-05 | 2017-04-27 | The United States Of America As Represented By The Secretary Of Agriculture | Methods for Synthesizing Graphene from a Lignin Source |
| US20180155201A1 (en) * | 2015-05-19 | 2018-06-07 | Key Team Enterprises Limited | Method for preparing graphene using coal as raw material |
| CA3005011A1 (en) * | 2018-02-14 | 2018-10-08 | United States Of America As Represented By The Secretary Of Agriculture | Lignin-based carbon foams and composites and related methods |
-
2019
- 2019-01-03 CN CN201910004249.2A patent/CN109437168B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20170113936A1 (en) * | 2013-06-05 | 2017-04-27 | The United States Of America As Represented By The Secretary Of Agriculture | Methods for Synthesizing Graphene from a Lignin Source |
| CN103466613A (en) * | 2013-10-11 | 2013-12-25 | 中南林业科技大学 | Method for preparing graphene from lignin |
| US20180155201A1 (en) * | 2015-05-19 | 2018-06-07 | Key Team Enterprises Limited | Method for preparing graphene using coal as raw material |
| CN105217607A (en) * | 2015-08-22 | 2016-01-06 | 苏州正业昌智能科技有限公司 | A kind of graphene preparation method based on xylogen |
| CN105439135A (en) * | 2015-12-30 | 2016-03-30 | 成都新柯力化工科技有限公司 | Method for preparing graphene from lignin |
| CN106241780A (en) * | 2016-07-19 | 2016-12-21 | 华南理工大学 | A kind of method preparing Graphene for raw material with lignin |
| CA3005011A1 (en) * | 2018-02-14 | 2018-10-08 | United States Of America As Represented By The Secretary Of Agriculture | Lignin-based carbon foams and composites and related methods |
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