CN109052383A - A kind of technique of electroosmose process separation graphene oxide - Google Patents
A kind of technique of electroosmose process separation graphene oxide Download PDFInfo
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Abstract
The invention discloses a kind of techniques of electroosmose process separation graphene oxide, and 1g graphite is mixed in 250ml conical flask with the 23ml concentrated sulfuric acid, is stirred at room temperature for 24 hours；Under 40 DEG C of water bath conditions, 100mg NaNO is added into dimension shape bottle3, and 5min is stirred, make NaNO3It is sufficiently molten out-of-the-way；500mgKMnO is slowly added into conical flask4, stir 30min；3ml distilled water is added into conical flask, 3ml swallow distilled water is added again after waiting 5min, 40ml distilled water is added after waiting 5min, stirs 15min；Stop water-bath, 140ml distilled water and 10ml30%H are added into conical flask2O2；5min is stirred at room temperature, to terminate reaction；The invention not only fundamentally solves the problems, such as that graphene oxide is difficult to wash and separate, but also the graphene oxide layer of different-grain diameter rank can be obtained by adjusting the electrodialysis reaction solution of different electricity, the different systems of configuration, difference pH, it is a kind of scientific, environmentally friendly, efficient graphene oxide separating technology.
Description
Technical field
The present invention relates to new material preparation technical field, specially a kind of work of electroosmose process separation graphene oxide
Skill.
Background technique
In recent years, graphene industry obtained rapid development, and was applied to the every field such as electronics, aerospace, new energy.
During using the preparation of oxidation-reduction method graphene, the graphene oxide for obtaining nano-scale, and graphite oxide are first had to
Alkene from acid saline solns washing and separation be in current graphene industrial production one influence quality and quantity bottleneck problem,
Research in relation to its separation is many, and vast resources and energy have also been put on man power and material, has changed traditional graphite oxide
Alkene separation method.
Summary of the invention
The purpose of the present invention is to provide a kind of techniques of electroosmose process separation graphene oxide, to solve above-mentioned background skill
The problem of being proposed in art.
In order to solve the above technical problem, the present invention provides following technical solutions: a kind of electroosmose process separation graphite oxide
The technique of alkene, includes the following steps, step 1 prepares graphene oxide；Step 2 configures electrodialysis buffer solution；Step 3,
Electrodialysis reaction；Step 4, dispersion optimization；Step 5, final process:
Wherein in above-mentioned steps one, 1g graphite is mixed in 250ml conical flask with the 23ml concentrated sulfuric acid, is stirred at room temperature
24h；Under 40 DEG C of water bath conditions, 100mg NaNO is added into dimension shape bottle3, and 5min is stirred, make NaNO3It is sufficiently molten out-of-the-way；To cone
500mgKMnO is slowly added in shape bottle4, stir 30min；3ml distilled water is added into conical flask, is added again after waiting 5min
3ml swallow distilled water is added 40ml distilled water after waiting 5min, stirs 15min；Stop water-bath, 140ml distillation is added into conical flask
Water and 10ml30%H2O2；5min is stirred at room temperature, to terminate reaction；Using centrifuge, 10000 turns/min, 3min, with 5%
HCI solution washes twice, and is then washed with distilled water to neutrality；Obtained sediment is dispersed in 100ml distilled water, and
90Hz ultrasound 60min, water level is parallel with liquid level when ultrasonic, washs at once after ultrasound；By above-mentioned acquired solution, 5000 turns/min,
5min centrifugation, takes after supernatant liquor that 5000 turns/min, 5min are centrifuged twice again, and gained clear liquid is RGO solution；
Wherein in above-mentioned steps two, three 250mL volumetric flasks are washed and dried with distilled water, set of pH is used
Buffer reagent is cut off polybag and is poured into reagent respectively in three beakers cleaned with distilled water, then respectively to three beakers
Bottle in distilled water is added, and by polybag with distilled water flushing twice, solution is poured into beaker, is slowly stirred with glass bar,
So that solid matter dissolves, after solid matter is completely dissolved, about 10min is stood, solution is cooled to room temperature；Drawn using glass bar
Stream pours into solution in beaker in preprepared volumetric flask；Beaker is scrubbed with distilled water, and is poured into volumetric flask, to capacity
Distilled water is added in bottle, until liquid level recess point is tangent with 150ml, 200ml and 250ml graduation mark；Plug is covered, overturns and shakes repeatedly
It shakes；
Wherein in above-mentioned steps three, the oxidation stone that will be prepared in the electrodialysis buffer solution and step 1 prepared in step 2
The two sides of a container are respectively placed in black solution, centre is obstructed using special ceramics permeable membrane, applies vertical electric field, carries out electric osmose
Analysis reaction；
Wherein in above-mentioned steps four, reducing agent will be added in reaction gained graphene oxide in step 3, being made has
The graphene oxide of polymolecularity；
Wherein in above-mentioned steps five, takes out reaction product and be separated by solid-liquid separation, gained solid phase is washed and dried to get graphite oxide
Alkene solid product, liquid phase recycling are recycled after processing.
According to the above technical scheme, in the step 1, KMnO is added4Afterwards, reaction temperature control is at 45 DEG C or less.
According to the above technical scheme, in the step 1,5000 turns are difficult to obtain complete centrifugation product, therefore need drink more
Supernatant liquid centrifugation, until obtaining supernatant liquor.
According to the above technical scheme, in the step 3, dialysis membrane material 60~100nm of aperture.
According to the above technical scheme, the electrodialysis pH of buffer is extremely adjustable in 3.5~8.0, can configure different systems.
According to the above technical scheme, in the step 4, reducing agent is gallic acid.
According to the above technical scheme, in the step 5, liquid phase recovery and treatment method is the concentration according to alkali before seal pot
After the concentration adjustment of solution alkali, used as caustic solution circulation
Compared with prior art, the beneficial effects obtained by the present invention are as follows being: the invention not only fundamentally solves oxidation
Graphene is difficult to the problem of washing and separating, but also can by adjusting different electricity, the different systems of configuration, difference pH electricity
Dialysis reaction solution obtains the graphene oxide layer of different-grain diameter rank, is a kind of scientific, environmentally friendly, efficient graphene oxide point
Separating process.
Detailed description of the invention
Attached drawing is used to provide further understanding of the present invention, and constitutes part of specification, with reality of the invention
It applies example to be used to explain the present invention together, not be construed as limiting the invention.In the accompanying drawings:
Fig. 1 is process flow diagram of the invention.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Referring to Fig. 1, the present invention provides a kind of technical solution: a kind of technique of electroosmose process separation graphene oxide:
Embodiment 1:
This example demonstrates that electricity is 220C, electrodialysis buffer concentration is reaction process and knot of 75%, the pH for 8.0
Fruit:
A kind of technique of electroosmose process separation graphene oxide, includes the following steps, step 1 prepares graphene oxide；
Step 2 configures electrodialysis buffer solution；Step 3, electrodialysis reaction；Step 4, dispersion optimization；Step 5, final process:
Wherein in above-mentioned steps one, 1g graphite is mixed in 250ml conical flask with the 23ml concentrated sulfuric acid, is stirred at room temperature
24h；Under 40 DEG C of water bath conditions, 100mg NaNO is added into dimension shape bottle3, and 5min is stirred, make NaNO3It is sufficiently molten out-of-the-way；To cone
500mgKMnO is slowly added in shape bottle4, reaction temperature control is at 45 DEG C hereinafter, stirring 30min；3ml is added into conical flask to steam
3ml swallow distilled water is added after waiting 5min in distilled water again, and 40ml distilled water is added after waiting 5min, stirs 15min；Stop water-bath,
140ml distilled water and 10ml30%H are added into conical flask2O2；5min is stirred at room temperature, to terminate reaction；Use centrifugation
Machine, 10000 turns/min, 3min, it is washed twice with 5%HCI solution, is then washed with distilled water to neutrality；It will be obtained heavy
Starch is dispersed in 100ml distilled water, and 90Hz ultrasound 60min, and water level is parallel with liquid level when ultrasonic, is washed at once after ultrasound；
By above-mentioned acquired solution, 5000 turns/min, 5min centrifugation takes after supernatant liquor that 5000 turns/min, 5min are centrifuged twice again, gained
Clear liquid is RGO solution, and 5000 turns are difficult to obtain complete centrifugation product, therefore the supernatant liquids that drink is needed to be centrifuged more, until obtaining
Supernatant liquor；
Wherein in above-mentioned steps two, three 250mL volumetric flasks are washed and dried with distilled water, set of pH is used
Buffer reagent is cut off polybag and is poured into reagent respectively in three beakers cleaned with distilled water, then respectively to three beakers
Bottle in distilled water is added, and by polybag with distilled water flushing twice, solution is poured into beaker, is slowly stirred with glass bar,
So that solid matter dissolves, after solid matter is completely dissolved, about 10min is stood, solution is cooled to room temperature；Drawn using glass bar
Stream pours into solution in beaker in preprepared volumetric flask；Beaker is scrubbed with distilled water, and is poured into volumetric flask, to capacity
Distilled water is added in bottle, until liquid level recess point is tangent with graduation mark；Plug is covered, overturns and rocks repeatedly；
Wherein in above-mentioned steps three, the oxidation stone that will be prepared in the electrodialysis buffer solution and step 1 prepared in step 2
The two sides of a container are respectively placed in black solution, centre is obstructed using special ceramics permeable membrane, dialysis membrane material aperture 60~
100nm applies vertical electric field, carries out electrodialysis reaction；
Wherein in above-mentioned steps four, gallic acid will be added in reaction gained graphene oxide in step 3, tool has been made
There is the graphene oxide of polymolecularity；
Wherein in above-mentioned steps five, takes out reaction product and be separated by solid-liquid separation, gained solid phase is washed and dried to get graphite oxide
Alkene solid product, liquid phase recycling are recycled after processing, and liquid phase recovery and treatment method is the concentration pair according to alkali before seal pot
After the concentration adjustment of solution alkali, used as caustic solution circulation.
Embodiment 2:
This example demonstrates that electricity is 180C, electrodialysis buffer concentration is reaction process and knot of 50%, the pH for 6.0
Fruit:
A kind of technique of electroosmose process separation graphene oxide, includes the following steps, step 1 prepares graphene oxide；
Step 2 configures electrodialysis buffer solution；Step 3, electrodialysis reaction；Step 4, dispersion optimization；Step 5, final process:
Wherein in above-mentioned steps one, 1g graphite is mixed in 250ml conical flask with the 23ml concentrated sulfuric acid, is stirred at room temperature
24h；Under 40 DEG C of water bath conditions, 100mg NaNO is added into dimension shape bottle3, and 5min is stirred, make NaNO3It is sufficiently molten out-of-the-way；To cone
500mgKMnO is slowly added in shape bottle4, reaction temperature control is at 45 DEG C hereinafter, stirring 30min；3ml is added into conical flask to steam
3ml swallow distilled water is added after waiting 5min in distilled water again, and 40ml distilled water is added after waiting 5min, stirs 15min；Stop water-bath,
140ml distilled water and 10ml30%H are added into conical flask2O2；5min is stirred at room temperature, to terminate reaction；Use centrifugation
Machine, 10000 turns/min, 3min, it is washed twice with 5%HCI solution, is then washed with distilled water to neutrality；It will be obtained heavy
Starch is dispersed in 100ml distilled water, and 90Hz ultrasound 60min, and water level is parallel with liquid level when ultrasonic, is washed at once after ultrasound；
By above-mentioned acquired solution, 5000 turns/min, 5min centrifugation takes after supernatant liquor that 5000 turns/min, 5min are centrifuged twice again, gained
Clear liquid is RGO solution, and 5000 turns are difficult to obtain complete centrifugation product, therefore the supernatant liquids that drink is needed to be centrifuged more, until obtaining
Supernatant liquor；
Wherein in above-mentioned steps two, three 250mL volumetric flasks are washed and dried with distilled water, set of pH is used
Buffer reagent is cut off polybag and is poured into reagent respectively in three beakers cleaned with distilled water, then respectively to three beakers
Bottle in distilled water is added, and by polybag with distilled water flushing twice, solution is poured into beaker, is slowly stirred with glass bar,
So that solid matter dissolves, after solid matter is completely dissolved, about 10min is stood, solution is cooled to room temperature；Drawn using glass bar
Stream pours into solution in beaker in preprepared volumetric flask；Beaker is scrubbed with distilled water, and is poured into volumetric flask, to capacity
Distilled water is added in bottle, until liquid level recess point is tangent with graduation mark；Plug is covered, overturns and rocks repeatedly；
Wherein in above-mentioned steps three, the oxidation stone that will be prepared in the electrodialysis buffer solution and step 1 prepared in step 2
The two sides of a container are respectively placed in black solution, centre is obstructed using special ceramics permeable membrane, dialysis membrane material aperture 60~
100nm applies vertical electric field, carries out electrodialysis reaction；
Wherein in above-mentioned steps four, gallic acid will be added in reaction gained graphene oxide in step 3, tool has been made
There is the graphene oxide of polymolecularity；
Wherein in above-mentioned steps five, takes out reaction product and be separated by solid-liquid separation, gained solid phase is washed and dried to get graphite oxide
Alkene solid product, liquid phase recycling are recycled after processing, and liquid phase recovery and treatment method is the concentration pair according to alkali before seal pot
After the concentration adjustment of solution alkali, used as caustic solution circulation.
Embodiment 3:
This example demonstrates that electricity is 120C, electrodialysis buffer concentration is reaction process and knot of 25%, the pH for 3.5
Fruit:
A kind of technique of electroosmose process separation graphene oxide, includes the following steps, step 1 prepares graphene oxide；
Step 2 configures electrodialysis buffer solution；Step 3, electrodialysis reaction；Step 4, dispersion optimization；Step 5, final process:
Wherein in above-mentioned steps one, 1g graphite is mixed in 250ml conical flask with the 23ml concentrated sulfuric acid, is stirred at room temperature
24h；Under 40 DEG C of water bath conditions, 100mg NaNO is added into dimension shape bottle3, and 5min is stirred, make NaNO3It is sufficiently molten out-of-the-way；To cone
500mgKMnO is slowly added in shape bottle4, reaction temperature control is at 45 DEG C hereinafter, stirring 30min；3ml is added into conical flask to steam
3ml swallow distilled water is added after waiting 5min in distilled water again, and 40ml distilled water is added after waiting 5min, stirs 15min；Stop water-bath,
140ml distilled water and 10ml30%H are added into conical flask2O2；5min is stirred at room temperature, to terminate reaction；Use centrifugation
Machine, 10000 turns/min, 3min, it is washed twice with 5%HCI solution, is then washed with distilled water to neutrality；It will be obtained heavy
Starch is dispersed in 100ml distilled water, and 90Hz ultrasound 60min, and water level is parallel with liquid level when ultrasonic, is washed at once after ultrasound；
By above-mentioned acquired solution, 5000 turns/min, 5min centrifugation takes after supernatant liquor that 5000 turns/min, 5min are centrifuged twice again, gained
Clear liquid is RGO solution, and 5000 turns are difficult to obtain complete centrifugation product, therefore the supernatant liquids that drink is needed to be centrifuged more, until obtaining
Supernatant liquor；
Wherein in above-mentioned steps two, three 250mL volumetric flasks are washed and dried with distilled water, set of pH is used
Buffer reagent is cut off polybag and is poured into reagent respectively in three beakers cleaned with distilled water, then respectively to three beakers
Bottle in distilled water is added, and by polybag with distilled water flushing twice, solution is poured into beaker, is slowly stirred with glass bar,
So that solid matter dissolves, after solid matter is completely dissolved, about 10min is stood, solution is cooled to room temperature；Drawn using glass bar
Stream pours into solution in beaker in preprepared volumetric flask；Beaker is scrubbed with distilled water, and is poured into volumetric flask, to capacity
Distilled water is added in bottle, until liquid level recess point is tangent with graduation mark；Plug is covered, overturns and rocks repeatedly；
Wherein in above-mentioned steps three, the oxidation stone that will be prepared in the electrodialysis buffer solution and step 1 prepared in step 2
The two sides of a container are respectively placed in black solution, centre is obstructed using special ceramics permeable membrane, dialysis membrane material aperture 60~
100nm applies vertical electric field, carries out electrodialysis reaction；
Wherein in above-mentioned steps four, gallic acid will be added in reaction gained graphene oxide in step 3, tool has been made
There is the graphene oxide of polymolecularity；
Wherein in above-mentioned steps five, takes out reaction product and be separated by solid-liquid separation, gained solid phase is washed and dried to get graphite oxide
Alkene solid product, liquid phase recycling are recycled after processing, and liquid phase recovery and treatment method is the concentration pair according to alkali before seal pot
After the concentration adjustment of solution alkali, used as caustic solution circulation.
Based on above-mentioned, it is an advantage of the current invention that it is of the invention, it not only fundamentally solves graphene oxide and is difficult to wash
The problem of with separation, but also can be obtained by adjusting the electrodialysis reaction solution of different electricity, the different systems of configuration, difference pH
The graphene oxide layer of different-grain diameter rank is a kind of scientific, environmentally friendly, efficient graphene oxide separating technology.
It should be noted that, in this document, relational terms such as first and second and the like are used merely to a reality
Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation
In any actual relationship or order or sequence.Moreover, the terms "include", "comprise" or its any other variant are intended to
Non-exclusive inclusion, so that the process, method, article or equipment including a series of elements is not only wanted including those
Element, but also including other elements that are not explicitly listed, or further include for this process, method, article or equipment
Intrinsic element.
Finally, it should be noted that the foregoing is only a preferred embodiment of the present invention, it is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features.
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in of the invention
Within protection scope.
Claims (7)
1. a kind of technique of electroosmose process separation graphene oxide, includes the following steps, step 1 prepares graphene oxide；Step
Rapid two, configure electrodialysis buffer solution；Step 3, electrodialysis reaction；Step 4, dispersion optimization；Step 5, final process,
It is characterized in that:
Wherein in above-mentioned steps one, 1g graphite is mixed in 250ml conical flask with the 23ml concentrated sulfuric acid, is stirred at room temperature for 24 hours；
Under 40 DEG C of water bath conditions, 100mg NaNO is added into dimension shape bottle3, and 5min is stirred, make NaNO3It is sufficiently molten out-of-the-way；To conical flask
In be slowly added to 500mgKMnO4, stir 30min；3ml distilled water is added into conical flask, 3ml is added again after waiting 5min
Swallow distilled water is added 40ml distilled water after waiting 5min, stirs 15min；Stop water-bath, 140ml distilled water is added into conical flask
And 10ml30%H2O2；5min is stirred at room temperature, to terminate reaction；Using centrifuge, 10000 turns/min, 3min, with 5%
HCI solution washes twice, and is then washed with distilled water to neutrality；Obtained sediment is dispersed in 100ml distilled water, and
90Hz ultrasound 60min, water level is parallel with liquid level when ultrasonic, washs at once after ultrasound；By above-mentioned acquired solution, 5000 turns/min,
5min centrifugation, takes after supernatant liquor that 5000 turns/min, 5min are centrifuged twice again, and gained clear liquid is RGO solution；
Wherein in above-mentioned steps two, three 250mL volumetric flasks are washed and dried with distilled water, are buffered using set of pH
Reagent is cut off polybag and is poured into reagent respectively in three beakers cleaned with distilled water, then respectively into three beaker bottles
Be added distilled water, and by polybag with distilled water flushing twice, solution is poured into beaker, is slowly stirred with glass bar so that
Solid matter dissolution stands about 10min after solid matter is completely dissolved, and solution is cooled to room temperature；Being drained using glass bar will
Solution pours into preprepared volumetric flask in beaker；Beaker is scrubbed with distilled water, and is poured into volumetric flask, into volumetric flask
Distilled water is added, until liquid level recess point is tangent with 150ml, 200ml and 250ml graduation mark；Plug is covered, overturns and rocks repeatedly；
It is wherein in above-mentioned steps three, the graphite oxide prepared in the electrodialysis buffer solution and step 1 prepared in step 2 is molten
The two sides of a container are respectively placed in liquid, centre is obstructed using special ceramics permeable membrane, applies vertical electric field, and it is anti-to carry out electrodialysis
It answers；
Wherein in above-mentioned steps four, reducing agent will be added in reaction gained graphene oxide in step 3, being made has high score
Dissipate the graphene oxide of property；
Wherein in above-mentioned steps five, takes out reaction product and be separated by solid-liquid separation, gained solid phase is washed and dry solid to get graphene oxide
Body product, liquid phase recycling are recycled after processing.
2. a kind of technique of electroosmose process separation graphene oxide according to claim 1, it is characterised in that: the step
In one, KMnO is added4Afterwards, reaction temperature control is at 45 DEG C or less.
3. a kind of technique of electroosmose process separation graphene oxide according to claim 1, it is characterised in that: the step
In one, 5000 turns are difficult to obtain complete centrifugation product, therefore the supernatant liquids that drink is needed to be centrifuged more, until obtaining supernatant liquor.
4. a kind of technique of electroosmose process separation graphene oxide according to claim 1, it is characterised in that: the step
In three, dialysis membrane material 60~100nm of aperture.
5. a kind of technique of electroosmose process separation graphene oxide according to claim 1, it is characterised in that: the electric osmose
It is extremely adjustable in 3.5~8.0 to analyse pH of buffer, can configure different systems.
6. a kind of technique of electroosmose process separation graphene oxide according to claim 1, it is characterised in that: the step
In four, reducing agent is gallic acid.
7. a kind of technique of electroosmose process separation graphene oxide according to claim 1, it is characterised in that: the step
In five, liquid phase recovery and treatment method is after being adjusted according to the concentration of alkali before seal pot to the concentration of solution alkali, to follow as aqueous slkali
Ring uses.
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Application publication date: 20181221 |