CN115448304A - Method for preparing graphene oxide in high-safety efficient water bath - Google Patents
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Abstract
The invention belongs to the technical field of graphene, and particularly relates to a method for preparing graphene oxide in a high-safety efficient water bath. The method for preparing graphene oxide adopted by the invention is to prepare graphene by cooling intercalation firstly and then water bath to assist in realizing closed oxidation stripping. The graphene oxide obtained by the method has an independent lamellar structure, compared with other physical methods, the method can effectively improve the stripping efficiency of graphite, compared with other chemical methods, toxic gas cannot overflow in the reaction process of the method, meanwhile, the method is simple to operate and high in safety in a sealed environment, and the prepared graphene oxide has the advantages of high yield, high yield and the like. The method with high safety is proved to be a method for preparing graphene oxide which can be widely popularized.
Description
Technical Field
The invention belongs to the technical field of graphene, and particularly relates to a method for preparing graphene oxide in a high-safety efficient water bath.
Background
Graphene, a new material with sp hybridized connected carbon atoms tightly packed into a single-layer two-dimensional honeycomb lattice structure. The graphene has excellent optical, electrical and mechanical properties, has important application prospects in the aspects of materials science, micro-nano processing, energy, biomedicine, drug delivery and the like, and is considered to be a revolutionary material in the future.
Common methods for producing graphene powder are a mechanical stripping method, an oxidation-reduction method and a SiC epitaxial growth method. However, the mechanical stripping method usually has difficulty in obtaining a thin layer of graphene oxide, and has a low yield and a long reaction time. The SiC epitaxial growth method can obtain high-quality graphene, but the method has higher requirements on equipment and higher product cost. The redox method is to fully oxidize graphite by a strong oxidant and the like to realize stripping of graphene oxide, the quality of the graphene oxide product obtained by the method is generally uniform and stable, and the stripping rate of the graphene oxide is high, but the chemical method needs to heat and stir oxidant such as concentrated sulfuric acid, sodium nitrate, potassium permanganate and the like at a high temperature (98 ℃), so that the method has great danger.
Therefore, the method for preparing the graphene oxide with high safety, high universality and high yield is researched, so that the safe and efficient preparation of the graphene oxide is realized, and the method has important significance.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a method for preparing graphene oxide by a closed oxidation method with high safety, high universality and high yield. The method disclosed by the invention is high in safety and simple to operate, and can be used for preparing the graphene oxide in a mass production manner.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing graphene oxide in a high-safety and high-efficiency water bath specifically comprises the following steps:
(1) The washed and thoroughly dried utensils such as a high borosilicate glass sealed tank, a measuring cylinder and the like, and raw materials such as concentrated sulfuric acid, potassium permanganate, hydrogen peroxide, graphite and the like required in the preparation process are fully dried and then placed in a refrigerator with the temperature of 0 ℃, and the constant temperature cooling is carried out for more than 4h for standby.
(2) Weighing graphite 1-5 g, adding into a high borosilicate glass sealed tank, weighing fully cooled concentrated sulfuric acid, pouring along the wall of a beaker, sealing, placing in ice water, and stirring for 1-2 h. Weighing a certain amount of potassium permanganate, slowly adding into the solution in batches, sealing and fully stirring for 2-4 h.
(3) Transferring the cooled high borosilicate glass sealed tank to a water bath kettle at 80 ℃, and keeping the constant temperature of 2-4 h. Naturally cooling at room temperature, transferring the obtained purple substance into a 1000mL beaker by using a glass rod, slowly adding 800mL deionized water, and uniformly stirring to obtain a brown dispersion liquid. And adding 5mL of 30% hydrogen peroxide solution, continuously stirring, changing the dispersion into bright yellow, and naturally settling for multiple times and washing with distilled water to obtain a black graphene oxide dispersion.
The proportion of the graphite, the concentrated sulfuric acid and the potassium permanganate is as follows: (0.5-5.0) g: (30-150) mL: (3.0-15.0) g.
The obtained graphene oxide shows good ultrathin layers and relatively complete graphene layer internal structures through tests such as SEM and Raman. The prepared graphene oxide is of a two-dimensional layered structure.
The graphite raw material may be natural graphite (crystalline graphite, graphite powder, expandable graphite) and artificial graphite (expanded graphite).
The required container of reaction is sealed container, and sealed safety protection, the environment of giving the minute-pressure that provides, including borosilicate glass seal jar, ceramic seal jar, polytetrafluoroethylene seal jar.
The method for preparing the graphene oxide is to realize closed oxidation stripping of the graphene by cooling intercalation firstly and then assisting in water bath. The graphene oxide obtained by the method has an independent lamellar structure, compared with other physical methods, the method can effectively improve the stripping efficiency of graphite, compared with other chemical methods, the method does not release toxic gas in the reaction process, and meanwhile, the method is simple to operate and high in safety in a sealed environment, and the prepared graphene oxide has the advantages of high yield, high yield and the like. The method with high safety is proved to be a method for preparing graphene oxide which can be widely popularized.
Advantageous effects
The invention discloses a method for preparing graphene oxide in a high-safety efficient water bath, which has the following advantages:
(1) The method for preparing the graphene oxide is simple and convenient to operate, complex instruments are not needed, only a high borosilicate glass sealed tank is adopted, the safety of the preparation process is greatly improved, and the yield of the graphene oxide is also improved.
(2) The water bath assists the oxidation stripping to be always carried out in a closed environment, and high safety is provided.
(3) The water bath assists the oxidation stripping to be constantly stirred, so that the oxidation stripping is fully carried out.
(4) The water bath assisted oxidation stripping process cancels a high-temperature reaction stage (98 ℃) which is necessary to be carried out by other chemical methods for preparing the graphene oxide, the water bath temperature is only about 80 ℃, the danger of rapid volume expansion possibly occurring under the high-temperature condition is thoroughly avoided, and the operation safety is ensured.
(5) The low-temperature stirring and water bath processes do not need manual participation, and complicated processes such as centrifugation and suction filtration can be thoroughly avoided in the subsequent treatment process of the sample, so that the contact between experimenters and strong oxidants can be effectively reduced, and the safety is fully improved.
(6) Other chemical reagents are not needed to be added in the subsequent treatment process of the sample, and only natural sedimentation and repeated washing by distilled water are adopted, so that the complicated process is reduced, and the safety is improved.
Description of the drawings:
fig. 1 is an XRD pattern of graphene oxide prepared by the method of the present invention;
FIG. 2 is a Raman diagram of graphene oxide prepared by the method of the present invention;
fig. 3 is an SEM image of graphene oxide prepared by the method of the present invention.
Detailed Description
Hereinafter, the present invention will be described in detail. Before the description is made, it should be understood that the terms used in the present specification and the appended claims should not be construed as limited to general and dictionary meanings, but interpreted based on the meanings and concepts corresponding to technical aspects of the present invention on the basis of the principle that the inventor is allowed to define terms appropriately for the best explanation. Accordingly, the description proposed herein is just a preferable example for the purpose of illustrations only, not intended to limit the scope of the invention, so it should be understood that other equivalents and modifications could be made thereto without departing from the spirit and scope of the invention.
The following examples are given by way of illustration of embodiments of the invention and are not to be construed as limiting the invention, and it will be understood by those skilled in the art that modifications may be made without departing from the spirit and scope of the invention. Unless otherwise specified, reagents and equipment used in the following examples are commercially available products.
Example 1
A method for preparing graphene oxide in a high-safety and high-efficiency water bath specifically comprises the following steps:
(1) Thoroughly drying vessels such as 300mL borosilicate glass sealed tanks, measuring cylinders and the like after being cleaned and concentrated sulfuric acid (H) required in the preparation process 2 SO 4 ) Potassium permanganate (KMnO) 4 ) And Expanded Graphite (EG) and other raw materials are fully dried and then placed in a refrigerator with the temperature of 0 ℃ and cooled for more than 4 hours at constant temperature for standby.
(2) Weighing 1g of expanded graphite, adding the expanded graphite into a high borosilicate glass sealed tank of 300mL, weighing fully-cooled 80ml of concentrated sulfuric acid, pouring the concentrated sulfuric acid along the wall of a beaker, sealing, placing the beaker in ice water and stirring for 1.5 hours. 5.0g of potassium permanganate is weighed and slowly added into the solution in batches, and the solution is sealed and fully stirred for 3 hours.
(3) The cooled high borosilicate glass sealed pot is transferred to a water bath kettle at 80 ℃, and the constant temperature is kept at 2h. Naturally cooling at room temperature, transferring the obtained purple substance into a 1000mL beaker by using a glass rod, slowly adding 800mL deionized water, and uniformly stirring to obtain a brown dispersion liquid. Adding 5mL of 30% hydrogen peroxide (H) 2 O 2 ) And continuously stirring the solution to change the dispersion liquid into bright yellow, and obtaining the black graphene oxide dispersion liquid after multiple times of natural sedimentation and washing by distilled water.
The XRD pattern of the prepared graphene oxide is shown in figure 1, and the spectrum of the product in figure 1 is consistent with the standard spectrum.
The Raman map of the prepared graphene oxide is shown in fig. 2, and the product in fig. 2 is a standard graphene oxide Raman map.
The SEM image of the prepared graphene oxide is shown in FIG. 3, and it can be seen from FIG. 3 that the prepared graphene oxide is a two-dimensional layered structure, and has a good ultrathin layer and a relatively complete graphene layer inner structure
Example 2
A method for preparing graphene oxide in high-safety efficient water bath specifically comprises the following steps:
(1) The washed and thoroughly dried vessels such as 300mL borosilicate glass sealed tanks and measuring cylinders and raw materials such as concentrated sulfuric acid, potassium permanganate and expandable graphite which are needed in the preparation process are fully dried and then placed in a refrigerator with the temperature of 0 ℃ and are cooled for more than 4 hours at constant temperature for standby.
(2) Weighing 1g of expandable graphite, adding the expandable graphite into a 300mL high borosilicate glass sealed tank, weighing fully cooled 80mL of concentrated sulfuric acid, pouring the concentrated sulfuric acid along the wall of a beaker, sealing, placing the beaker in ice water, and stirring for 1.5 hours. 5.0g of potassium permanganate is weighed and slowly added into the solution in batches, and the solution is sealed and fully stirred for 3 hours.
(3) The cooled high borosilicate glass sealed pot is transferred to a water bath kettle at 80 ℃, and the constant temperature is kept at 2h. Naturally cooling at room temperature, transferring the purple substance into a 1000mL beaker by using a glass rod, slowly adding 800mL deionized water, and uniformly stirring to obtain a brown dispersion liquid. Adding 5mL of 30% hydrogen peroxide solution, continuously stirring, changing the dispersion liquid into bright yellow, and naturally settling for multiple times and washing with distilled water to obtain a black graphene oxide dispersion liquid.
Example 3
(1) The washed and thoroughly dried utensils such as 300mL high borosilicate glass sealed tanks, measuring cylinders and the like, and raw materials such as concentrated sulfuric acid, potassium permanganate and crystalline graphite which are needed to be used in the preparation process are fully dried and then placed in a refrigerator with the temperature of 0 ℃, and the cooled raw materials are cooled for more than 4 hours at constant temperature for standby.
(2) Weighing 1g of crystalline graphite, adding the crystalline graphite into a high borosilicate glass sealed tank of 300mL, weighing fully-cooled 80ml of concentrated sulfuric acid, pouring the concentrated sulfuric acid along the wall of a beaker, sealing, placing the beaker in ice water, and stirring for 1.5 hours. 5.0g of potassium permanganate is weighed and slowly added into the solution in batches, and the solution is sealed and fully stirred for 3 hours.
(3) The cooled high borosilicate glass sealed pot is transferred to a water bath kettle at 80 ℃, and the constant temperature is kept at 2h. After natural cooling at room temperature, the purple material was transferred to a 1000mL beaker using a glass rod, and 800mL deionized water was slowly added and stirred well to obtain a brown dispersion. Adding 5mL of 30% hydrogen peroxide solution, continuously stirring, changing the dispersion liquid into bright yellow, and obtaining the black graphene oxide dispersion liquid after multiple natural sedimentation and washing by distilled water.
Example 4
A method for preparing graphene oxide in a high-safety and high-efficiency water bath specifically comprises the following steps:
(1) The washed and thoroughly dried utensils such as 300mL high borosilicate glass sealed tanks, measuring cylinders and the like and raw materials such as concentrated sulfuric acid, potassium permanganate, graphite powder and the like required in the preparation process are fully dried and then placed in a refrigerator with the temperature of 0 ℃, and the cooled raw materials are cooled for more than 4 hours at constant temperature for standby.
(2) Weighing 1g of graphite powder, adding the graphite powder into a 300mL high borosilicate glass sealed tank, weighing fully-cooled 80mL of concentrated sulfuric acid, pouring the concentrated sulfuric acid along the wall of a beaker, sealing, placing the beaker in ice water, and stirring for 1.5 hours. 5.0g of potassium permanganate is weighed and slowly added into the solution in batches, and the solution is sealed and fully stirred for 3 hours.
(3) The cooled borosilicate glass sealed tank is transferred to a water bath kettle at 80 ℃, and the temperature is kept constant at 2h. After natural cooling at room temperature, the purple material was transferred to a 1000mL beaker using a glass rod, and 800mL deionized water was slowly added and stirred well to obtain a brown dispersion. Adding 5mL of 30% hydrogen peroxide solution, continuously stirring, changing the dispersion liquid into bright yellow, and naturally settling for multiple times and washing with distilled water to obtain a black graphene oxide dispersion liquid.
Example 5
A method for preparing graphene oxide in high-safety efficient water bath specifically comprises the following steps:
(1) The washed and thoroughly dried utensils such as 300mL high borosilicate glass sealed tanks, measuring cylinders and the like, and raw materials such as concentrated sulfuric acid, potassium permanganate and natural graphite which are needed to be used in the preparation process are fully dried and then placed in a refrigerator with the temperature of 0 ℃, and the raw materials are cooled for more than 4 hours at constant temperature for standby.
(2) Weighing 1g of natural graphite, adding the natural graphite into a 300mL high borosilicate glass sealed tank, weighing fully cooled 80mL of concentrated sulfuric acid, pouring the concentrated sulfuric acid along the wall of a beaker, sealing, placing the beaker in ice water, and stirring for 1.5 hours. 5.0g of potassium permanganate is weighed and slowly added into the solution in batches, and the solution is sealed and fully stirred for 3 hours.
(3) The cooled high borosilicate glass sealed pot is transferred to a water bath kettle at 80 ℃, and the constant temperature is kept at 2h. After natural cooling at room temperature, the purple material was transferred to a 1000mL beaker using a glass rod, and 800mL deionized water was slowly added and stirred well to obtain a brown dispersion. Adding 5mL of 30% hydrogen peroxide solution, continuously stirring, changing the dispersion liquid into bright yellow, and naturally settling for multiple times and washing with distilled water to obtain a black graphene oxide dispersion liquid.
Example 6
A method for preparing graphene oxide in high-safety efficient water bath specifically comprises the following steps:
(1) The method comprises the steps of washing, completely drying utensils such as 300ml high borosilicate glass sealed tanks and measuring cylinders and raw materials such as concentrated sulfuric acid, potassium permanganate and Expanded Graphite (EG) required in the preparation process, fully drying, placing in a refrigerator with the temperature of 0 ℃, and cooling at constant temperature for more than 4 hours for later use.
(2) Weighing 2g of expanded graphite, adding the expanded graphite into a 300mL high borosilicate glass sealed tank, weighing 160mL of fully cooled concentrated sulfuric acid, pouring the concentrated sulfuric acid along the wall of a beaker, sealing, placing the beaker in ice water, and stirring for 2 hours. Weighing 10g of potassium permanganate, slowly adding the potassium permanganate into the solution in batches, sealing and fully stirring for 4 hours.
(3) The cooled borosilicate glass sealed tank is transferred to a water bath kettle at 80 ℃, and the temperature is kept constant at 2h. After natural cooling at room temperature, the purple material was transferred to a 1000mL beaker using a glass rod, and 800mL deionized water was slowly added and stirred well to obtain a brown dispersion. Adding 10mL of 30% hydrogen peroxide solution, continuously stirring, changing the dispersion liquid into bright yellow, and naturally settling for multiple times and washing with distilled water to obtain black graphene oxide dispersion liquid.
Example 7
A method for preparing graphene oxide in a high-safety and high-efficiency water bath specifically comprises the following steps:
(1) The cleaned and thoroughly dried utensils such as 300ml high borosilicate glass sealed tanks, measuring cylinders and the like, and raw materials such as concentrated sulfuric acid, potassium permanganate and Expanded Graphite (EG) required in the preparation process are fully dried and then placed in a refrigerator with the temperature of 0 ℃, and the cooled raw materials are cooled for more than 4 hours at constant temperature for standby.
(2) Weighing 3g of expanded graphite, adding the expanded graphite into a 300mL high borosilicate glass sealed tank, weighing fully cooled 200mL of concentrated sulfuric acid, pouring the concentrated sulfuric acid along the wall of a beaker, sealing, placing the beaker in ice water, and stirring for 2 hours. 15g of potassium permanganate is weighed and slowly added into the solution in batches, and the solution is sealed and fully stirred for 4 hours.
(3) The cooled high borosilicate glass sealed pot is transferred to a water bath kettle at 80 ℃, and the constant temperature is kept at 2h. After natural cooling at room temperature, the purple material was transferred to a 1000mL beaker using a glass rod, and 800mL deionized water was slowly added and stirred well to obtain a brown dispersion. Adding 12mL of 30% hydrogen peroxide solution, continuously stirring, changing the dispersion liquid into bright yellow, and obtaining black graphene oxide dispersion liquid after multiple times of natural sedimentation and washing by distilled water.
Example 8
A method for preparing graphene oxide in high-safety efficient water bath specifically comprises the following steps:
(1) The washed and thoroughly dried vessels such as 500ml of high borosilicate glass sealed tanks, measuring cylinders and the like, and raw materials such as concentrated sulfuric acid, potassium permanganate, expanded Graphite (EG) and the like required in the preparation process are fully dried and then placed in a refrigerator with the temperature of 0 ℃, and the constant temperature cooling is carried out for more than 4 hours for standby.
(2) Weighing 5g of expanded graphite, adding the expanded graphite into a 500mL high borosilicate glass sealed tank, weighing fully cooled 400mL of concentrated sulfuric acid, pouring the concentrated sulfuric acid along the wall of a beaker, sealing, placing the beaker in ice water, and stirring for 2 hours. 25g of potassium permanganate is weighed and slowly added into the solution in batches, and the solution is sealed and fully stirred for 4 hours.
(3) The cooled high borosilicate glass sealed pot is transferred to a water bath kettle at 80 ℃, and the constant temperature is kept at 2h. After natural cooling at room temperature, the purple material was transferred to a 2000mL beaker using a glass rod, and 1600mL of deionized water was slowly added and stirred well to give a brown dispersion. Adding 20mL of 30% hydrogen peroxide solution, continuously stirring, changing the dispersion liquid into bright yellow, and obtaining black graphene oxide dispersion liquid after multiple times of natural sedimentation and washing by distilled water.
The above examples are only intended to illustrate the technical solution of the present invention, and not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions.
Claims (9)
1. A method for preparing graphene oxide in high-safety and high-efficiency water bath is characterized by comprising the following steps: (1) pretreatment: fully drying the vessel and the raw materials used in the reaction, and then cooling at constant temperature of 0 ℃ for more than 4 hours for later use;
(2) Low-temperature intercalation: adding graphite into a reaction container, adding fully cooled concentrated sulfuric acid, sealing the reaction container, and stirring at a low temperature to react for 1-2 h; adding potassium permanganate into the reaction solution, sealing the reaction container, and fully stirring for reaction for 2-4 h;
(3) Water bath heating oxidation stripping: heating the reaction system to 75-85 ℃, and stirring and reacting for 2-4 h at constant temperature;
(5) And (3) post-treatment: and naturally cooling at room temperature, slowly adding deionized water, uniformly stirring to obtain a brown dispersion, adding a 30% hydrogen peroxide solution, continuously stirring to obtain a bright yellow dispersion, and naturally settling for multiple times and washing with distilled water to obtain a black graphene oxide dispersion.
2. The method for preparing graphene oxide through high-safety high-efficiency water bath according to claim 1, wherein the prepared graphene oxide is of a two-dimensional layered structure.
3. The method for preparing graphene oxide through high-safety high-efficiency water bath according to claim 2, wherein the prepared graphene oxide has an independent lamellar structure.
4. The method for preparing graphene oxide through high-safety high-efficiency water bath according to claim 1, wherein the graphite raw material is one or more of crystalline graphite, graphite powder, expandable graphite and expanded graphite.
5. The method for preparing graphene oxide through high-safety high-efficiency water bath according to claim 1, wherein the reaction vessel is one of a high borosilicate glass sealed tank, a ceramic sealed tank and a polytetrafluoroethylene sealed tank.
6. The method for preparing graphene oxide through high-safety high-efficiency water bath according to claim 1, wherein in the step (2), the reaction vessel is sealed and stirred in an ice-water mixture for reaction.
7. The method for preparing graphene oxide through high-safety high-efficiency water bath according to claim 1, wherein in the step (3), the reaction system is heated to 80 ℃ through the water bath, and is stirred and reacted at a constant temperature of 80 ℃.
8. The method for preparing graphene oxide through a high-safety high-efficiency water bath according to claim 7, wherein in the step (3), the reaction vessel is sealed during the water bath reaction, so that a micro-pressure environment is provided.
9. The method for preparing graphene oxide through high-safety high-efficiency water bath according to claim 1, wherein the proportion of the graphite to the concentrated sulfuric acid to the potassium permanganate is as follows: (0.5-5.0) g: (30-150) mL: (3.0-15.0) g.
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