CN108946714A - The method that green, quick magnanimity prepares graphene oxide - Google Patents
The method that green, quick magnanimity prepares graphene oxide Download PDFInfo
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- CN108946714A CN108946714A CN201811029168.XA CN201811029168A CN108946714A CN 108946714 A CN108946714 A CN 108946714A CN 201811029168 A CN201811029168 A CN 201811029168A CN 108946714 A CN108946714 A CN 108946714A
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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
- C01B32/19—Preparation by exfoliation
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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
- C01B32/198—Graphene oxide
Abstract
The method that green, quick magnanimity prepares graphene oxide, it is related to a kind of method for preparing graphene oxide, is related to preparing the preparation field of graphene oxide.The present invention is to solve existing the technical issues of preparing graphene oxide pollution environment.This method is as follows: one, preparation can extruding micro-nano graphite；Two, graphene oxide dispersion is prepared；Three, it is 5% progress reduction reaction that reduced sugar to reduction Sugar concentration is added into graphene oxide dispersion, moisture is steamed under the conditions of temperature is 150 DEG C~200 DEG C or decomposes organic medium, vacuum freeze drying is carried out in -50 DEG C of cold-trap again, obtains graphene powder.Reaction time of the invention is short, and preparation speed is fast, is not only able to obtain graphene oxide rapidly in the case where low power consuming, and introduces without having to worry about other impurities, and operation is simple, and technical process is cheap.
Description
Technical field
The present invention relates to a kind of method for preparing graphene oxide, it is related to preparing the preparation field of graphene oxide.
Background technique
So far from graphene discovery, domestic and international experts and scholars constantly explore in terms of the preparation and application of graphene always,
There are a variety of methods that can obtain grapheme material at present.Nearly 3 years, with the continuous development of graphene technology and industry,
Mainly using physical method and chemical method preparation and production graphene, however the most common method for preparing graphene is to use to improve
Hummers method oxidation processes carried out to natural flake graphite prepare graphite oxide, through ultrasonic disperse, obtain graphene oxide point
Then dispersion liquid heats reduction under the action of the reducing agents such as hydrazine hydrate-ethylene glycol, finally obtains graphene.Even if by going back by force
After former agent reduction, the prototype structure of graphene can not be restored completely, and make its electronic structure and perfection of crystal by
Serious destruction, and a large amount of waste liquids are generated during extraction, and product is largely lost with waste liquid, cause environmental pollution and
Economic loss.
Summary of the invention
The purpose of the present invention is to solve existing the technical issues of preparing graphene oxide pollution environment, provide one kind
The method that green, quick magnanimity prepares graphene oxide.
The method that green, quick magnanimity prepares graphene oxide follows the steps below:
One, the high-purity natural crystalline flake graphite after cleaning dust is applied into 60MPa pressure under conditions of temperature is 25 DEG C,
Object block after molding is put into the mixed solution of oxalic acid, sulfuric acid, propene carbonate and Li salt by rapid shaping, is taken after impregnating 2h
Out, expanding treatment 15min is carried out in the case where power is the microwave of 1500W, the product after expanding treatment is separated from liquid, is obtained
Can extruding micro-nano graphite；
Two, by can the micro-nano graphite of extruding be put into aqueous medium or organic medium and impregnate 30min, then in 100W
Ultrasonic stripping off device in carry out ultrasound 1.5h, 90min after by liquid solid be centrifuged or filter remove, reservation liquid, obtain
Obtain uniform and stable bronzing graphene oxide dispersion；
Three, it is 5% progress reduction reaction that reduced sugar to reduction Sugar concentration is added into graphene oxide dispersion,
Temperature steams moisture under the conditions of being 150 DEG C~200 DEG C or decomposes organic medium, then vacuum is carried out in -50 DEG C of cold-trap
Freeze-drying, obtains graphene powder.
Li salt described in step 1 is one or more of lithium nitrate, lithium carbonate and lithium sulfate.
The purity of high-purity natural crystalline flake graphite described in step 1 is 99.9%.
Aqueous medium described in step 2 is deionized water.
Organic medium described in step 2 is ethyl alcohol or methanol.
The invention proposes a kind of quick, efficient, green preparation graphene oxide dispersion methods, by the oxidation of acquisition
Graphene dispersing solution reduction, can get graphene product.This method is using cheap natural flake graphite as raw material, through cold
After molded, obtained rapidly through microwave oxidizing process can the micro-nano graphite of extruding, then obtain a large amount of oxidation stones rapidly through step ultrasound
Black alkene dispersion liquid, and without considering liquid waste processing problem, toxic or pollution gas is not generated in preparation process, and raw material is honest and clean
Valence is easy to get, and has achieved the purpose that produce preparation process Green environmental protection and rapidly and efficiently, has been a kind of preparation method of green.
The technical solution adopted by the present invention to solve the technical problems is:
1. first by the washing of raw material high-purity natural crystalline flake graphite, drying, to remove the impurity such as dust, then through cold moudling
Expanding treatment is carried out, so that obtaining can the micro-nano graphite of extruding.
2. by acquisition can the micro-nano graphite of extruding, be added in the sonification medium of independent research, be subject to sonic oscillation, make it
It is evenly dispersed in the medium.
3. above-mentioned evenly dispersed liquid is made it be separated by solid-liquid separation or filter and separates, retain the liquid through high speed centrifugation,
For yellowish-brown graphene oxide dispersion, solid is recycled, further ultrasound, is repeated the above process, can constantly obtain yellowish-brown
The dispersion of color graphene oxide, graphene oxide dispersion can get graphene through restoring.
It is an advantage of the invention that the reaction time is short, preparation speed is fast, is not only able to obtain rapidly in the case where low power consuming
Graphene oxide, and introduced without having to worry about other impurities, operation is simple, and technical process is cheap.
Specific embodiment
The technical solution of the present invention is not limited to the following list, further includes between each specific embodiment
Any combination.
Specific embodiment 1: present embodiment Green, quick magnanimity prepare the method for graphene oxide according to following
Step carries out:
One, the high-purity natural crystalline flake graphite after cleaning dust is applied into 60MPa pressure under conditions of temperature is 25 DEG C,
Object block after molding is put into the mixed solution of oxalic acid, sulfuric acid, propene carbonate and Li salt by rapid shaping, is taken after impregnating 2h
Out, expanding treatment 15min is carried out in the case where power is the microwave of 1500W, the product after expanding treatment is separated from liquid, is obtained
Can extruding micro-nano graphite；
Two, by can the micro-nano graphite of extruding be put into aqueous medium or organic medium and impregnate 30min, then in 100W
Ultrasonic stripping off device in carry out ultrasound 1.5h, 90min after by liquid solid be centrifuged or filter remove, reservation liquid, obtain
Obtain uniform and stable bronzing graphene oxide dispersion；
Three, it is 5% progress reduction reaction that reduced sugar to reduction Sugar concentration is added into graphene oxide dispersion,
Temperature steams moisture under the conditions of being 150 DEG C~200 DEG C or decomposes organic medium, then vacuum is carried out in -50 DEG C of cold-trap
Freeze-drying, obtains graphene powder.
Specific embodiment 2: the present embodiment is different from the first embodiment in that oxalic acid described in step 1, sulphur
Acid, the mixed solution mesoxalic acid of propene carbonate and Li salt, sulfuric acid, propene carbonate and Li salt mass ratio be 2:3:5:1.Its
It is same as the specific embodiment one.
Specific embodiment 3: the present embodiment is different from the first and the second embodiment in that Li salt described in step 1
For one or more of lithium nitrate, lithium carbonate and lithium sulfate.It is other the same as one or two specific embodiments.
Specific embodiment 4: unlike one of present embodiment and specific embodiment one to three described in step 2
Aqueous medium is deionized water.It is other identical as one of specific embodiment one to three.
Specific embodiment 5: unlike one of present embodiment and specific embodiment one to four in step 2
The organic medium is ethyl alcohol or methanol.It is other identical as one of specific embodiment one to four.
Specific embodiment 6: unlike one of present embodiment and specific embodiment one to five in step 3
It is described to steam moisture under the conditions of temperature is 150 DEG C or decompose organic medium.It is other with specific embodiment one to five it
One is identical.
Specific embodiment 7: unlike one of present embodiment and specific embodiment one to six in step 3
It is described to steam moisture under the conditions of temperature is 160 DEG C or decompose organic medium.It is other with specific embodiment one to six it
One is identical.
Specific embodiment 8: unlike one of present embodiment and specific embodiment one to seven in step 3
It is described to steam moisture under the conditions of temperature is 170 DEG C or decompose organic medium.It is other with specific embodiment one to seven it
One is identical.
Specific embodiment 9: unlike one of present embodiment and specific embodiment one to eight in step 3
It is described to steam moisture under the conditions of temperature is 180 DEG C or decompose organic medium.It is other with specific embodiment one to eight it
One is identical.
Specific embodiment 10: unlike one of present embodiment and specific embodiment one to nine in step 3
It is described to steam moisture under the conditions of temperature is 190 DEG C or decompose organic medium.It is other with specific embodiment one to nine it
One is identical.
Effect of the present invention is verified using following embodiments:
Embodiment 1:
The method that green, quick magnanimity prepares graphene oxide follows the steps below:
One, the high-purity natural crystalline flake graphite after cleaning dust is applied into 60MPa pressure under conditions of temperature is 25 DEG C,
Object block after molding is put into the mixed solution of oxalic acid, sulfuric acid, propene carbonate and Li salt by rapid shaping, is taken after impregnating 2h
Out, expanding treatment 15min is carried out in the case where power is the microwave of 1500W, the product after expanding treatment is separated from liquid, is obtained
Can extruding micro-nano graphite；
Two, by can the micro-nano graphite of extruding be put into aqueous medium or organic medium and impregnate 30min, then in 100W
Ultrasonic stripping off device in carry out ultrasound 1.5h, 90min after by liquid solid be centrifuged or filter remove, reservation liquid, obtain
Obtain uniform and stable bronzing graphene oxide dispersion；
Three, it is 5% progress reduction reaction that reduced sugar to reduction Sugar concentration is added into graphene oxide dispersion,
Temperature steams moisture under the conditions of being 150 DEG C or decomposes organic medium, then carries out vacuum refrigeration in -50 DEG C of cold-trap and do
It is dry, obtain graphene powder.
Embodiment 2:
The method that green, quick magnanimity prepares graphene oxide follows the steps below:
One, the high-purity natural crystalline flake graphite after cleaning dust is applied into 60MPa pressure under conditions of temperature is 25 DEG C,
Object block after molding is put into the mixed solution of oxalic acid, sulfuric acid, propene carbonate and Li salt by rapid shaping, is taken after impregnating 2h
Out, expanding treatment 15min is carried out in the case where power is the microwave of 1500W, the product after expanding treatment is separated from liquid, is obtained
Can extruding micro-nano graphite；
Two, by can the micro-nano graphite of extruding be put into aqueous medium or organic medium and impregnate 30min, then in 100W
Ultrasonic stripping off device in carry out ultrasound 1.5h, 90min after by liquid solid be centrifuged or filter remove, reservation liquid, obtain
Obtain uniform and stable bronzing graphene oxide dispersion；
Three, it is 5% progress reduction reaction that reduced sugar to reduction Sugar concentration is added into graphene oxide dispersion,
Temperature steams moisture under the conditions of being 160 DEG C or decomposes organic medium, then carries out vacuum refrigeration in -50 DEG C of cold-trap and do
It is dry, obtain graphene powder.
Embodiment 3:
Hair growth composition the preparation method is as follows:
The method that green, quick magnanimity prepares graphene oxide follows the steps below:
One, the high-purity natural crystalline flake graphite after cleaning dust is applied into 60MPa pressure under conditions of temperature is 25 DEG C,
Object block after molding is put into the mixed solution of oxalic acid, sulfuric acid, propene carbonate and Li salt by rapid shaping, is taken after impregnating 2h
Out, expanding treatment 15min is carried out in the case where power is the microwave of 1500W, the product after expanding treatment is separated from liquid, is obtained
Can extruding micro-nano graphite；
Two, by can the micro-nano graphite of extruding be put into aqueous medium or organic medium and impregnate 30min, then in 100W
Ultrasonic stripping off device in carry out ultrasound 1.5h, 90min after by liquid solid be centrifuged or filter remove, reservation liquid, obtain
Obtain uniform and stable bronzing graphene oxide dispersion；
Three, it is 5% progress reduction reaction that reduced sugar to reduction Sugar concentration is added into graphene oxide dispersion,
Temperature steams moisture under the conditions of being 170 DEG C or decomposes organic medium, then carries out vacuum refrigeration in -50 DEG C of cold-trap and do
It is dry, obtain graphene powder.
Embodiment 4:
The method that green, quick magnanimity prepares graphene oxide follows the steps below:
One, the high-purity natural crystalline flake graphite after cleaning dust is applied into 60MPa pressure under conditions of temperature is 25 DEG C,
Object block after molding is put into the mixed solution of oxalic acid, sulfuric acid, propene carbonate and Li salt by rapid shaping, is taken after impregnating 2h
Out, expanding treatment 15min is carried out in the case where power is the microwave of 1500W, the product after expanding treatment is separated from liquid, is obtained
Can extruding micro-nano graphite；
Two, by can the micro-nano graphite of extruding be put into aqueous medium or organic medium and impregnate 30min, then in 100W
Ultrasonic stripping off device in carry out ultrasound 1.5h, 90min after by liquid solid be centrifuged or filter remove, reservation liquid, obtain
Obtain uniform and stable bronzing graphene oxide dispersion；
Three, it is 5% progress reduction reaction that reduced sugar to reduction Sugar concentration is added into graphene oxide dispersion,
Temperature steams moisture under the conditions of being 180 DEG C or decomposes organic medium, then carries out vacuum refrigeration in -50 DEG C of cold-trap and do
It is dry, obtain graphene powder.
Embodiment 5:
The method that green, quick magnanimity prepares graphene oxide follows the steps below:
One, the high-purity natural crystalline flake graphite after cleaning dust is applied into 60MPa pressure under conditions of temperature is 25 DEG C,
Object block after molding is put into the mixed solution of oxalic acid, sulfuric acid, propene carbonate and Li salt by rapid shaping, is taken after impregnating 2h
Out, expanding treatment 15min is carried out in the case where power is the microwave of 1500W, the product after expanding treatment is separated from liquid, is obtained
Can extruding micro-nano graphite；
Two, by can the micro-nano graphite of extruding be put into aqueous medium or organic medium and impregnate 30min, then in 100W
Ultrasonic stripping off device in carry out ultrasound 1.5h, 90min after by liquid solid be centrifuged or filter remove, reservation liquid, obtain
Obtain uniform and stable bronzing graphene oxide dispersion；
Three, it is 5% progress reduction reaction that reduced sugar to reduction Sugar concentration is added into graphene oxide dispersion,
Temperature steams moisture under the conditions of being 190 DEG C or decomposes organic medium, then carries out vacuum refrigeration in -50 DEG C of cold-trap and do
It is dry, obtain graphene powder.
Embodiment 6:
The method that green, quick magnanimity prepares graphene oxide follows the steps below:
One, the high-purity natural crystalline flake graphite after cleaning dust is applied into 60MPa pressure under conditions of temperature is 25 DEG C,
Object block after molding is put into the mixed solution of oxalic acid, sulfuric acid, propene carbonate and Li salt by rapid shaping, is taken after impregnating 2h
Out, expanding treatment 15min is carried out in the case where power is the microwave of 1500W, the product after expanding treatment is separated from liquid, is obtained
Can extruding micro-nano graphite；
Two, by can the micro-nano graphite of extruding be put into aqueous medium or organic medium and impregnate 30min, then in 100W
Ultrasonic stripping off device in carry out ultrasound 1.5h, 90min after by liquid solid be centrifuged or filter remove, reservation liquid, obtain
Obtain uniform and stable bronzing graphene oxide dispersion；
Three, it is 5% progress reduction reaction that reduced sugar to reduction Sugar concentration is added into graphene oxide dispersion,
Temperature steams moisture under the conditions of being 200 DEG C or decomposes organic medium, then carries out vacuum refrigeration in -50 DEG C of cold-trap and do
It is dry, obtain graphene powder.
Claims (10)
1. the method that green, quick magnanimity prepare graphene oxide, it is characterised in that green, quick magnanimity prepares graphene oxide
Method follow the steps below:
One, the high-purity natural crystalline flake graphite after cleaning dust is applied into 60MPa pressure, quickly under conditions of temperature is 25 DEG C
Molding, object block after molding is put into the mixed solution of oxalic acid, sulfuric acid, propene carbonate and Li salt, is taken out after impregnating 2h,
Expanding treatment 15min is carried out under the microwave that power is 1500W, the product after expanding treatment is separated from liquid, acquisition can be swollen
The micro-nano graphite changed；
Two, by can the micro-nano graphite of extruding be put into aqueous medium or organic medium and impregnate 30min, then in the super of 100W
The solid in liquid is centrifuged or is filtered removal after carrying out ultrasound 1.5h, 90min in sound stripping off device, retains liquid, is obtained equal
Even stable bronzing graphene oxide dispersion；
Three, it is 5% progress reduction reaction that reduced sugar to reduction Sugar concentration is added into graphene oxide dispersion, in temperature
Moisture is steamed under the conditions of being 150 DEG C~200 DEG C or decomposes organic medium, then vacuum refrigeration is carried out in -50 DEG C of cold-trap
It is dry, obtain graphene powder.
2. the method that green, quick magnanimity prepare graphene oxide according to claim 1, it is characterised in that institute in step 1
The mass ratio for stating the mixed solution mesoxalic acid of oxalic acid, sulfuric acid, propene carbonate and Li salt, sulfuric acid, propene carbonate and Li salt is
2:3:5:1。
3. the method that green, quick magnanimity prepare graphene oxide according to claim 1, it is characterised in that institute in step 1
Stating Li salt is one or more of lithium nitrate, lithium carbonate and lithium sulfate.
4. the method that green, quick magnanimity prepare graphene oxide according to claim 1, it is characterised in that institute in step 2
Stating aqueous medium is deionized water.
5. the method that green, quick magnanimity prepare graphene oxide according to claim 1, it is characterised in that institute in step 2
Stating organic medium is ethyl alcohol or methanol.
6. the method that green, quick magnanimity prepare graphene oxide according to claim 1, it is characterised in that institute in step 3
It states and steams moisture under the conditions of temperature is 150 DEG C or decompose organic medium.
7. the method that green, quick magnanimity prepare graphene oxide according to claim 1, it is characterised in that institute in step 3
It states and steams moisture under the conditions of temperature is 160 DEG C or decompose organic medium.
8. the method that green, quick magnanimity prepare graphene oxide according to claim 1, it is characterised in that institute in step 3
It states and steams moisture under the conditions of temperature is 170 DEG C or decompose organic medium.
9. the method that green, quick magnanimity prepare graphene oxide according to claim 1, it is characterised in that institute in step 3
It states and steams moisture under the conditions of temperature is 180 DEG C or decompose organic medium.
10. the method that green, quick magnanimity prepare graphene oxide according to claim 1, it is characterised in that in step 3
It is described to steam moisture under the conditions of temperature is 190 DEG C or decompose organic medium.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112547463A (en) * | 2020-11-14 | 2021-03-26 | 广东中晨电子科技有限公司 | High-performance graphene composite aluminum sheet and preparation method and application thereof |
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Application publication date: 20181207 |