CN106957053A - A kind of iron powder is the method for the quick macroscopic preparation of graphene of reducing agent - Google Patents
A kind of iron powder is the method for the quick macroscopic preparation of graphene of reducing agent Download PDFInfo
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- CN106957053A CN106957053A CN201710239803.6A CN201710239803A CN106957053A CN 106957053 A CN106957053 A CN 106957053A CN 201710239803 A CN201710239803 A CN 201710239803A CN 106957053 A CN106957053 A CN 106957053A
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- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
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- C01B2204/32—Size or surface area
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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- Y02P20/10—Process efficiency
Abstract
The present invention relates to new material technology field, a kind of method that iron powder is the quick macroscopic preparation of graphene of reducing agent is particularly disclosed.The iron powder is the method for the quick macroscopic preparation of graphene of reducing agent, it is characterised in that：Graphite oxide is prepared using improved Hummers methods, oxidation product, ultrasonically treated rear vibration or strong stirring is diluted with pure water, obtains graphene oxide acid solution；Graphene oxide acid solution is transferred in reaction vessel, reproducibility iron powder is added after heating, cooling is stood after reaction, is filtered, graphene powder is made in scrubbed, dry, crushing, screening.The reducing agent for the redox graphene that the present invention is selected is reproducibility iron powder, and cheap, nontoxic pollution-free belongs to environmentally friendly reagent；Graphene preparation process energy consumption is low, the cycle is short, pollution is small, it is adaptable to large-scale production.
Description
（One）Technical field
The present invention relates to new material technology field, more particularly to a kind of iron powder is the side of the quick macroscopic preparation of graphene of reducing agent
Method.
（Two）Background technology
Graphene（graphene）It is the Two-dimensional Carbon atomic crystal of monoatomic thickness, it is considered to be constitute fullerene, CNT
With the basic structural unit of graphite.In nature, graphene is most thin a kind of material that people are recognized, its thickness is only
For 0.335nm.Its atomic arrangement is as monoatomic layer graphite, and it is numerous peculiar that the structure of this almost Perfect has graphene
The performance such as electricity, calorifics, mechanics.Its thermal conductivity good (5000W/ (mK), the big (2630m of specific surface area2/ g), carrier is dense
Degree is up to 1013/cm2, electron mobility is up to 2 × 10 at room temperature5cm2/(V·s).Excellent performance causes graphene in chemistry
There is light in the fields such as energy storage, sensor, electrically conductive ink, heat sink material, anticorrosive paint, functional rubber, sewage disposal, desalinization
Bright application prospect.
At present, preparing the method for graphene mainly has mechanical stripping method, vapour deposition process, epitaxial growth method, arc process, electricity
Chemical method, organic synthesis method and reducing process etc..Wherein graphene oxide reducing process is because its is with low cost and preparation process is relatively simple
It is single, it is the unique effective way for preparing grapheme material on a large scale at present.At present, redox graphene mainly has high warm also
Former method and chemical reduction method.But this two classes method has shortcoming, first kind method reaction temperature is high, high energy consumption, and equipment will
Ask high；Equations of The Second Kind method, for example pure hydrazine hydrate of conventional chemical reducing agent, sodium borohydride etc. are poisonous, easily pollute environment.Therefore, open
It is efficient to send out a kind of, green, cheap graphene preparation method be graphene and graphene-based composite property further investigation and
Wide variety of premise.
（Three）The content of the invention
The present invention is reducing agent to make up the deficiencies in the prior art there is provided the iron powder of a kind of low cost, low energy consumption, low stain
The method of quick macroscopic preparation of graphene.
The present invention is achieved through the following technical solutions：
A kind of iron powder is the method for the quick macroscopic preparation of graphene of reducing agent, is comprised the following steps：
（1）Graphite oxide is prepared using improved Hummers methods, oxidation product is diluted with pure water, is stirred through ultrasound, vibration or strength
Processing is mixed, graphene oxide acid solution is obtained；
（2）Graphene oxide acid solution is transferred in reaction vessel, is warming up under 40-98 DEG C, stirring condition, reproducibility iron is added
Powder, reacts 1-6h, and standing is cooled to 50 DEG C, filtered while hot, and graphene powder is made in scrubbed, dry, crushing, screening.
The present invention prepares graphite oxide using improved Hummers methods, and graphite oxide is handled to obtain through dilution and ultrasonic disperse
Olefin(e) acid liquid, then prepares graphene with iron powder reducing graphene oxide.Compared with traditional reducing agent, with industrialized reproducibility
Iron powder is as reducing agent, and raw material is cheap, nontoxic.In addition, iron powder reducing graphene oxide, process energy consumption is low, pollute less, the cycle
It is short, it is easy to which that rapid batch prepares graphene, be conducive to promoting graphene in chemical energy storage, sensor, electrically conductive ink, radiating material
The application in the fields such as material, anticorrosive paint, functional rubber, sewage disposal, desalinization.
The present invention more excellent technique effect be：
Step（1）In, the improved Hummers methods of use, including improved all methods based on Hummers methods.
Step（1）In, reaction product adds pure water to be diluted to 0.1-5mg/ml, preferably 0.5-2mg/ml；It is ultrasonically treated preferred
2-3h；Ultrasonic power is 100W-10KW, preferably 2-5KW；Vibration or strong stirring 1-2h.
Step（2）In, the mass ratio of reducing agent iron powder and graphene oxide is 1-10:1, preferably 2-4:1.
Step（2）In, acidic oxidation graphene acid solution is warming up to 60-90 DEG C；Reproducibility iron powder is added, 2-3h is reacted.
Step（2）In, washing step is first to be washed with 3-10wt% watery hydrochloric acid, then washed with pure water；Drying mode is freezing
Dry, oven drying or spray drying；Grinding mode is air-flow crushing or mechanical crushing.
The reducing agent for the redox graphene that the present invention is selected is reproducibility iron powder, cheap, nontoxic pollution-free, category
In environmentally friendly reagent；Graphene preparation process energy consumption is low, the cycle is short, pollution is small, it is adaptable to large-scale production.
（Four）Brief description of the drawings
The present invention is further illustrated below in conjunction with the accompanying drawings.
Fig. 1 is the X-ray diffracting spectrum of the graphene of the gained of the embodiment of the present invention 1（XRD）；
Fig. 2 is the scanning electron microscope diagram of the graphene of the gained of the embodiment of the present invention 1（SEM）；
Fig. 3 is the transmission electron microscope figure of the graphene of the gained of the embodiment of the present invention 1（TEM）.
（Five）Embodiment
Embodiment 1：A kind of restoring method of graphene oxide, comprises the following steps：
（1）The preparation of graphene oxide：Using improve Hummers methods prepare graphite oxide, first, by 20g native graphites and by
The 0.6L mixed acid of 0.54 concentrated sulfuric acid and 0.06L concentrated phosphoric acids composition is mixed in reactor, opens magnetic stirrer uniform.
Temperature of charge is slowly added to 80g potassium permanganate in the case of being less than 20 DEG C in kettle；80 DEG C are warming up to afterwards to react 2 hours, will
Product is discharged, and is added 6 times of deionization pure water dilution, is added the graphite oxide acid solution that glassy yellow is made in hydrogen peroxide；Continue to add
Water is diluted to 0.56mg/ml, the ultrasonically treated 1h of 3KW, obtains graphene oxide acid solution；
（2）The preparation of graphene：Graphene oxide acid solution is transferred in reactor, under the conditions of electric stirring, 90 DEG C are warming up to,
Add at 128g iron powder, 90 DEG C and react 3h；Then, the iron powder for removing residual is washed with 5% watery hydrochloric acid, then pure water is washed till filtrate
PH=7, is finally freeze-dried, and graphene powder is made in mechanical crushing, screening.Understood through analysis test：Graphene electricity after reduction
Conductance is 2895S/m, and specific surface area is 163m2/g。
Embodiment 2：A kind of restoring method of graphene oxide, comprises the following steps：
（1）The preparation of graphite oxide：Using improve Hummers methods prepare graphite oxide, first, by 20g native graphites and by
The 0.6L mixed acid of 0.54 concentrated sulfuric acid and 0.06L concentrated phosphoric acids composition is mixed in reactor, opens magnetic stirrer uniform.
Temperature of charge is slowly added to 80g potassium permanganate in the case of being less than 20 DEG C in kettle；80 DEG C are warming up to afterwards to react 2 hours, will
Product is discharged, and is added 6 times of deionization pure water dilution, is added the graphite oxide acid solution that glassy yellow is made in hydrogen peroxide；Continue to add
Water is diluted to 0.56mg/ml, the ultrasonically treated 1h of 3KW, obtains graphene oxide acid solution；
（2）The preparation of graphene：Graphene oxide acid solution is transferred in reactor, under the conditions of electric stirring, 90 DEG C are warming up to,
256g iron powder is added, 1h is reacted at 90 DEG C；Then the iron powder for removing residual is washed with 5% watery hydrochloric acid, then pure water is washed till filtrate
PH=7, is finally freeze-dried, and graphene powder is made in mechanical crushing, screening.Understood through analysis test：Graphene electricity after reduction
Conductance is 2755S/m, and specific surface area is 195m2/g。
Embodiment 3：
（1）The preparation of graphene oxide：Using improve Hummers methods prepare graphite oxide, first, by 200g native graphites and by
The 6L mixed acid of 5.4 concentrated sulfuric acids and 0.6L concentrated phosphoric acids composition is mixed in reactor, opens magnetic stirrer uniform.In kettle
Interior temperature of charge is slowly added to 800g potassium permanganate in the case of being less than 20 DEG C；It is warming up to 80 DEG C afterwards to react 1 hour, by product
Discharge, adds pure water and is diluted to 40L, adds the graphite oxide acid solution that glassy yellow is made in 0.2L hydrogen peroxide；Then pure water is added
It is diluted to 0.45mg/ml；Measure 60L, 0.45mg/ml graphite oxide and hang suspension, the ultrasonically treated 2h of 600W obtain graphene oxide
Acid solution；
（2）The preparation of graphene：Graphene oxide acid solution is transferred in 100L reactors, 90 DEG C are warming up under electric stirring,
Then 128g iron powder, 90 DEG C of reaction 1h are added；Then, the iron powder for removing residual is washed with 10wt% watery hydrochloric acid, then pure water is washed till
Filtrate pH=7, most obtains graphene powder through high shear, spray drying, air-flow crushing, screening afterwards.Through analysis test：Graphene powder
Bulk conductivity is 2598S/m, and specific surface area is 286m2/g。
Embodiment 4：
（1）The preparation of graphene oxide：Using improve Hummers methods prepare graphite oxide, first, by 200g native graphites and by
The 6L mixed acid of 5.4 concentrated sulfuric acids and 0.6L concentrated phosphoric acids composition is mixed in reactor, opens magnetic stirrer uniform.In kettle
Interior temperature of charge is slowly added to 800g potassium permanganate in the case of being less than 20 DEG C；It is warming up to 80 DEG C afterwards to react 1 hour, by product
Discharge, adds pure water and is diluted to 40L, adds the graphite oxide acid solution that glassy yellow is made in 0.2L hydrogen peroxide；Then pure water is added
It is diluted to 0.45mg/ml；Measure 60L, 0.45mg/ml graphite oxide and hang suspension, the ultrasonically treated 2h of 600W obtain graphene oxide
Acid solution；
（2）The preparation of graphene：Graphene oxide acid solution is transferred in 100L reactors, 90 DEG C are warming up under electric stirring,
Then 128g iron powder, 90 DEG C of reaction 3h are added；Then, the iron powder for removing residual is washed with 5wt% watery hydrochloric acid, then pure water is washed till
Filtrate pH=7, most obtains graphene powder through high shear, spray drying, air-flow crushing, screening afterwards.Through analysis test：Graphene powder
Bulk conductivity is 3450S/m, and specific surface area is 180m2/g。
Embodiment 5：
（1）The preparation of graphene oxide：Using improve Hummers methods prepare graphite oxide, first, by 200g native graphites and by
The 6L mixed acid of 5.4 concentrated sulfuric acids and 0.6L concentrated phosphoric acids composition is mixed in reactor, opens magnetic stirrer uniform.In kettle
Interior temperature of charge is slowly added to 800g potassium permanganate in the case of being less than 20 DEG C；It is warming up to 80 DEG C afterwards to react 1 hour, by product
Discharge, adds pure water and is diluted to 40L, adds the graphite oxide acid solution that glassy yellow is made in 0.2L hydrogen peroxide；Then pure water is added
It is diluted to 0.45mg/ml；Measure 60L, 0.45mg/ml graphite oxide and hang suspension, the ultrasonically treated 6h of 600W obtain graphene oxide
Acid solution；
（2）The preparation of graphene：Graphene oxide acid solution is transferred in 100L reactors, 90 DEG C are warming up under electric stirring,
Then 128g iron powder, 90 DEG C of reaction 1h are added；Then, the iron powder for removing residual is washed with 5wt% watery hydrochloric acid, then pure water is washed till
Filtrate pH=7, most obtains graphene powder through high shear, spray drying, air-flow crushing, screening afterwards.Through analysis test：Graphene powder
Bulk conductivity is 3096S/m, and specific surface area is 235m2/g。
Embodiment 6：
（1）The preparation of graphene oxide：Using improve Hummers methods prepare graphite oxide, first, by 200g native graphites and by
The 6L mixed acid of 5.4 concentrated sulfuric acids and 0.6L concentrated phosphoric acids composition is mixed in reactor, opens magnetic stirrer uniform.In kettle
Interior temperature of charge is slowly added to 800g potassium permanganate in the case of being less than 20 DEG C；It is warming up to 80 DEG C afterwards to react 1 hour, by product
Discharge, adds pure water and is diluted to 40L, adds the graphite oxide acid solution that glassy yellow is made in 0.2L hydrogen peroxide；Then pure water is added
It is diluted to 0.45mg/ml；Measure 60L, 0.45mg/ml graphite oxide and hang suspension, the ultrasonically treated 2h of 600W obtain graphene oxide
Acid solution；
（2）The preparation of graphene：Graphene oxide acid solution is transferred in 100L reactors, 50 DEG C are warming up under electric stirring,
Then 128g iron powder, 50 DEG C of reaction 3h are added；Then, the iron powder for removing residual is washed with 5wt% watery hydrochloric acid, then pure water is washed till
Filtrate pH=7, most obtains graphene powder through high shear, spray drying, air-flow crushing, screening afterwards.Through analysis test：Graphene powder
Bulk conductivity is 2547S/m, and specific surface area is 258m2/g。
Embodiment 7：
（1）The preparation of graphene oxide：Using improve Hummers methods prepare graphite oxide, first, by 200g native graphites and by
The 6L mixed acid of 5.4 concentrated sulfuric acids and 0.6L concentrated phosphoric acids composition is mixed in reactor, opens magnetic stirrer uniform.In kettle
Interior temperature of charge is slowly added to 800g potassium permanganate in the case of being less than 20 DEG C；It is warming up to 80 DEG C afterwards to react 1 hour, by product
Discharge, adds pure water and is diluted to 40L, adds the graphite oxide acid solution that glassy yellow is made in 0.2L hydrogen peroxide；Then pure water is added
It is diluted to 0.45mg/ml；Measure 60L, 0.45mg/ml graphite oxide and hang suspension, the ultrasonically treated 2h of 600W obtain graphene oxide
Acid solution；
（2）The preparation of graphene：Graphene oxide acid solution is transferred in 100L reactors, 70 DEG C are warming up under electric stirring,
Then 128g iron powder, 70 DEG C of reaction 3h are added；Then, the iron powder for removing residual is washed with 5wt% watery hydrochloric acid, then pure water is washed till
Filtrate pH=7, most obtains graphene powder through high shear, spray drying, air-flow crushing, screening afterwards.Through analysis test：Graphene powder
Bulk conductivity is 2679S/m, and specific surface area is 226m2/g。
Embodiment 8：
（1）The preparation of graphene oxide：Using improve Hummers methods prepare graphite oxide, first, by 200g native graphites and by
The 6L mixed acid of 5.4 concentrated sulfuric acids and 0.6L concentrated phosphoric acids composition is mixed in reactor, opens magnetic stirrer uniform.In kettle
Interior temperature of charge is slowly added to 800g potassium permanganate in the case of being less than 20 DEG C；It is warming up to 80 DEG C afterwards to react 1 hour, by product
Discharge, adds pure water and is diluted to 40L, adds the graphite oxide acid solution that glassy yellow is made in 0.2L hydrogen peroxide；Then pure water is added
It is diluted to 0.45mg/ml；Measure 60L, 0.45mg/ml graphite oxide and hang suspension, the ultrasonically treated 2h of 600W obtain graphene oxide
Acid solution；
（2）The preparation of graphene：Graphene oxide acid solution is transferred in 100L reactors, 90 DEG C are warming up under electric stirring,
Then 64g iron powder, 90 DEG C of reaction 3h are added；Then, the iron powder for removing residual is washed with 5wt% watery hydrochloric acid, then pure water is washed till filter
Liquid pH=7, most obtains graphene powder through high shear, spray drying, air-flow crushing, screening afterwards.Through analysis test：Graphene powder
Electrical conductivity is 2435S/m, and specific surface area is 253m2/g。
Claims (9)
1. a kind of iron powder is the method for the quick macroscopic preparation of graphene of reducing agent, it is characterized in that, comprise the following steps：（1）Using
Improved Hummers methods prepare graphite oxide, and oxidation product is diluted with pure water, are handled through ultrasound, vibration or strong stirring, obtain oxygen
Graphite olefin(e) acid liquid；（2）Graphene oxide acid solution is transferred in reaction vessel, is warming up under 40-98 DEG C, stirring condition, plus
Enter reproducibility iron powder, react 1-6h, standing is cooled to 50 DEG C, filtered while hot, graphite is made in scrubbed, dry, crushing, screening
Alkene powder.
2. iron powder according to claim 1 is the method for the quick macroscopic preparation of graphene of reducing agent, it is characterised in that：Step
（1）In, reaction product adds pure water to be diluted to 0.1-5mg/ml, and ultrasonically treated 2-3h, ultrasonic power is 100W-10KW, vibration or
Strong stirring 1-2h.
3. iron powder according to claim 1 is the method for the quick macroscopic preparation of graphene of reducing agent, it is characterised in that：Step
（2）In, the mass ratio of reducing agent iron powder and graphene oxide is 1-10:1.
4. iron powder according to claim 1 is the method for the quick macroscopic preparation of graphene of reducing agent, it is characterised in that：Step
（2）In, acidic oxidation graphene acid solution is warming up to 60-90 DEG C, adds reproducibility iron powder, reacts 2-3h.
5. iron powder according to claim 1 is the method for the quick macroscopic preparation of graphene of reducing agent, it is characterised in that：Step
（2）In, washing step is first to be washed with 3-10wt% watery hydrochloric acid, then washed with pure water.
6. iron powder according to claim 1 is the method for the quick macroscopic preparation of graphene of reducing agent, it is characterised in that：Step
（2）In, drying mode is freeze-drying, oven drying or spray drying.
7. iron powder according to claim 1 is the method for the quick macroscopic preparation of graphene of reducing agent, it is characterised in that：Step
（2）In, grinding mode is air-flow crushing or mechanical crushing.
8. iron powder according to claim 2 is the method for the quick macroscopic preparation of graphene of reducing agent, it is characterised in that：Step
（1）In, reaction product adds pure water to be diluted to 0.5-2mg/ml, and ultrasonic power is 2-5KW.
9. iron powder according to claim 3 is the method for the quick macroscopic preparation of graphene of reducing agent, it is characterised in that：Step
（2）In, the mass ratio of reducing agent iron powder and graphene oxide is 2-4:1.
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Cited By (1)
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| CN109678140A (en) * | 2018-12-07 | 2019-04-26 | 中国环境科学研究院 | A kind of green modified carbon nano tube material and its preparation method and application |
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