CN108217638A - A kind of method for the redox graphene for preparing activation of potassium hydroxide - Google Patents
A kind of method for the redox graphene for preparing activation of potassium hydroxide Download PDFInfo
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- CN108217638A CN108217638A CN201810308387.5A CN201810308387A CN108217638A CN 108217638 A CN108217638 A CN 108217638A CN 201810308387 A CN201810308387 A CN 201810308387A CN 108217638 A CN108217638 A CN 108217638A
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Abstract
A kind of method for the redox graphene for preparing activation of potassium hydroxide, including：Step 1：5g graphite, 1g sodium nitrate are weighed, 2 grams of potassium nitrate and 2 grams of sodium bicarbonates are placed in the beaker of 1000mL, the 150mL concentrated sulfuric acids are slowly added into beaker, beaker is placed in ice-water bath, magnetic agitation 1h;Step 2：Weigh 15g potassium permanganate and 2 grams of sodium permanganates, be slowly added in beaker and be stirred continuously, keep in beaker mixture temperature 30 DEG C hereinafter, beaker to be placed in room temperature later under be stirred continuously for 24 hours.
Description
Technical field
The present invention relates to a kind of methods for the redox graphene for preparing activation of potassium hydroxide.
Background technology
The method flow of the redox graphene of the prior art for preparing activation of potassium hydroxide is complicated, low precision, no
Environmental protection.
Invention content
A kind of method for the redox graphene for preparing activation of potassium hydroxide, including：
Step 1：5g graphite is weighed, 1g sodium nitrate, 2 grams of potassium nitrate and 2 grams of sodium bicarbonates are placed in the beaker of 1000mL, to beaker
In be slowly added to the 150mL concentrated sulfuric acids, beaker is placed in ice-water bath, magnetic agitation 1h;
Step 2：15g potassium permanganate and 2 grams of sodium permanganates are weighed, is slowly added in beaker and is stirred continuously, keep mixing in beaker
Close object temperature 30 DEG C hereinafter, beaker to be placed in room temperature later under be stirred continuously for 24 hours;
Step 3：Beaker is placed in ice-water bath, be slowly added to 300mL deionized waters and is stirred continuously, keeps mixture in beaker
Temperature is at 98 DEG C hereinafter, being then slowly added into the aqueous hydrogen peroxide solution that 30mL mass fractions are 30% and being stirred continuously;
Step 4：Mixed solution is packed into centrifuge tube, 30min is centrifuged under 8000rpm, supernatant liquid is removed, sediment is taken
Go out, wash and centrifuged 6 times with the aqueous hydrochloric acid solution that volume fraction is 10%, sediment is taken out to be placed in bag filter carry out by a definite date 3
The dialysis in week obtains graphite oxide suspension to remove salt ion and acid ion completely;
Step 5：Graphite oxide suspension is scattered in deionized water, configuration quality score is the suspension of 1mg/mL, to it
Ultrasonic disperse processing is carried out, ultrasonic time 1h centrifuges 30min and removes unstripped graphite oxide at 3,000 rpm, final to obtain
To graphene oxide aqueous dispersions；
Step 6：Using graphene oxide aqueous dispersions made from step 5, configuration concentration is the graphene oxide water of 0.3mg/mL
Dispersion liquid takes 500mL graphene oxide aqueous dispersions to be placed in three-neck flask；
Step 7：Three-neck flask is fixed on iron stand, middle port and side neck mouth with glass stopper are covered tightly, pass through opposite side
It is molten that neck mouth adds in the hydrazine that the ammonium hydroxide that 1mL mass fractions are 28wt.% and 80 μ L mass fractions are 80wt.% into three-neck flask
Then liquid also covers tightly this side port with glass stopper, and carry out abundant magnetic agitation；
Step 8：Spiral coil cooling tube is placed on the interstitial hole of three-neck flask, cooling water is opened and fills coiled pipe and keep water outlet
Flow in small thread shape, adjust the position of iron stand geometrical clamp, three-neck flask be placed in 95 DEG C of oil bath and reacts 1h,
Period keeps sufficient magnetic agitation, after completion of the reaction takes out three-neck flask from oil bath；
Step 9：After cooled to room temperature, the black suspension in bottle is filtered to remove in draught cupboard after three-neck flask
It removes to swim in apparent large stretch of carbon-coating on liquid level, redox graphene is obtained after then suspension is filtered and dried；
Step 10：Using redox graphene made from step 9 as raw material, configuration concentration is the redox graphene of 5mg/mL
Aqueous solution 40mL is placed in the plastic bottle that capacity is 60mL, the potassium hydroxide solution of point a concentration of 6mol/L of addition 3mL, abundant magnetic
Power stirs 2h and places 12h after sealing under room temperature；
Step 11：Mixed liquor made from step 10 is subjected to freeze-drying 72h at -55 DEG C；
Step 12：Sample after freeze-drying is placed in tube furnace, is heat-treated under argon gas atmosphere protection：First to pipe
Formula stove carries out vacuum pumping, and setting heating rate is 20 DEG C/min, and target temperature is 800 DEG C, soaking time 30min, argon
Throughput is 400sccm, and operating air pressure 100Pa cools to room temperature with the furnace after reaction；
Step 13：The product of step 12 is washed 2 times, then be washed with deionized with the aqueous hydrochloric acid solution that volume fraction is 10%
It is about 7 to pH value, product is freeze-dried, obtains the redox graphene of activation of potassium hydroxide.
The redox graphene of the activation of potassium hydroxide of the present invention can be applied to super capacitor.
Inventive point is：1）Complete reaction process；2）Material used；3）Concrete component.
Specific embodiment
Embodiment 1
A kind of method for the redox graphene for preparing activation of potassium hydroxide, including：
Step 1：5g graphite is weighed, 1g sodium nitrate, 2 grams of potassium nitrate and 2 grams of sodium bicarbonates are placed in the beaker of 1000mL, to beaker
In be slowly added to the 150mL concentrated sulfuric acids, beaker is placed in ice-water bath, magnetic agitation 1h;
Step 2：15g potassium permanganate and 2 grams of sodium permanganates are weighed, is slowly added in beaker and is stirred continuously, keep mixing in beaker
Close object temperature 30 DEG C hereinafter, beaker to be placed in room temperature later under be stirred continuously for 24 hours;
Step 3：Beaker is placed in ice-water bath, be slowly added to 300mL deionized waters and is stirred continuously, keeps mixture in beaker
Temperature is at 98 DEG C hereinafter, being then slowly added into the aqueous hydrogen peroxide solution that 30mL mass fractions are 30% and being stirred continuously;
Step 4：Mixed solution is packed into centrifuge tube, 30min is centrifuged under 8000rpm, supernatant liquid is removed, sediment is taken
Go out, wash and centrifuged 6 times with the aqueous hydrochloric acid solution that volume fraction is 10%, sediment is taken out to be placed in bag filter carry out by a definite date 3
The dialysis in week obtains graphite oxide suspension to remove salt ion and acid ion completely;
Step 5：Graphite oxide suspension is scattered in deionized water, configuration quality score is the suspension of 1mg/mL, to it
Ultrasonic disperse processing is carried out, ultrasonic time 1h centrifuges 30min and removes unstripped graphite oxide at 3,000 rpm, final to obtain
To graphene oxide aqueous dispersions；
Step 6：Using graphene oxide aqueous dispersions made from step 5, configuration concentration is the graphene oxide water of 0.3mg/mL
Dispersion liquid takes 500mL graphene oxide aqueous dispersions to be placed in three-neck flask；
Step 7：Three-neck flask is fixed on iron stand, middle port and side neck mouth with glass stopper are covered tightly, pass through opposite side
It is molten that neck mouth adds in the hydrazine that the ammonium hydroxide that 1mL mass fractions are 28wt.% and 80 μ L mass fractions are 80wt.% into three-neck flask
Then liquid also covers tightly this side port with glass stopper, and carry out abundant magnetic agitation；
Step 8：Spiral coil cooling tube is placed on the interstitial hole of three-neck flask, cooling water is opened and fills coiled pipe and keep water outlet
Flow in small thread shape, adjust the position of iron stand geometrical clamp, three-neck flask be placed in 95 DEG C of oil bath and reacts 1h,
Period keeps sufficient magnetic agitation, after completion of the reaction takes out three-neck flask from oil bath；
Step 9：After cooled to room temperature, the black suspension in bottle is filtered to remove in draught cupboard after three-neck flask
It removes to swim in apparent large stretch of carbon-coating on liquid level, redox graphene is obtained after then suspension is filtered and dried；
Step 10：Using redox graphene made from step 9 as raw material, configuration concentration is the redox graphene of 5mg/mL
Aqueous solution 40mL is placed in the plastic bottle that capacity is 60mL, the potassium hydroxide solution of point a concentration of 6mol/L of addition 3mL, abundant magnetic
Power stirs 2h and places 12h after sealing under room temperature；
Step 11：Mixed liquor made from step 10 is subjected to freeze-drying 72h at -55 DEG C；
Step 12：Sample after freeze-drying is placed in tube furnace, is heat-treated under argon gas atmosphere protection：First to pipe
Formula stove carries out vacuum pumping, and setting heating rate is 20 DEG C/min, and target temperature is 800 DEG C, soaking time 30min, argon
Throughput is 400sccm, and operating air pressure 100Pa cools to room temperature with the furnace after reaction；
Step 13：The product of step 12 is washed 2 times, then be washed with deionized with the aqueous hydrochloric acid solution that volume fraction is 10%
It is about 7 to pH value, product is freeze-dried, obtains the redox graphene of activation of potassium hydroxide.
The redox graphene of the activation of potassium hydroxide of the present invention can be applied to super capacitor.
Embodiment 2
A kind of method for the redox graphene for preparing activation of potassium hydroxide, including：
Step 1：5g graphite is weighed, 1g sodium nitrate, 2 grams of potassium nitrate and 2.2 grams of sodium bicarbonates are placed in the beaker of 1000mL, to burning
The 150mL concentrated sulfuric acids are slowly added in cup, beaker are placed in ice-water bath, magnetic agitation 1h;
Step 2：15g potassium permanganate and 2 grams of sodium permanganates are weighed, is slowly added in beaker and is stirred continuously, keep mixing in beaker
Close object temperature 30 DEG C hereinafter, beaker to be placed in room temperature later under be stirred continuously for 24 hours;
Step 3：Beaker is placed in ice-water bath, be slowly added to 300mL deionized waters and is stirred continuously, keeps mixture in beaker
Temperature is at 98 DEG C hereinafter, being then slowly added into the aqueous hydrogen peroxide solution that 30mL mass fractions are 30% and being stirred continuously;
Step 4：Mixed solution is packed into centrifuge tube, 30min is centrifuged under 8000rpm, supernatant liquid is removed, sediment is taken
Go out, wash and centrifuged 6 times with the aqueous hydrochloric acid solution that volume fraction is 10%, sediment is taken out to be placed in bag filter carry out by a definite date 3
The dialysis in week obtains graphite oxide suspension to remove salt ion and acid ion completely;
Step 5：Graphite oxide suspension is scattered in deionized water, configuration quality score is the suspension of 1mg/mL, to it
Ultrasonic disperse processing is carried out, ultrasonic time 1h centrifuges 30min and removes unstripped graphite oxide at 3,000 rpm, final to obtain
To graphene oxide aqueous dispersions；
Step 6：Using graphene oxide aqueous dispersions made from step 5, configuration concentration is the graphene oxide water of 0.3mg/mL
Dispersion liquid takes 500mL graphene oxide aqueous dispersions to be placed in three-neck flask；
Step 7：Three-neck flask is fixed on iron stand, middle port and side neck mouth with glass stopper are covered tightly, pass through opposite side
It is molten that neck mouth adds in the hydrazine that the ammonium hydroxide that 1mL mass fractions are 28wt.% and 80 μ L mass fractions are 80wt.% into three-neck flask
Then liquid also covers tightly this side port with glass stopper, and carry out abundant magnetic agitation；
Step 8：Spiral coil cooling tube is placed on the interstitial hole of three-neck flask, cooling water is opened and fills coiled pipe and keep water outlet
Flow in small thread shape, adjust the position of iron stand geometrical clamp, three-neck flask be placed in 95 DEG C of oil bath and reacts 1h,
Period keeps sufficient magnetic agitation, after completion of the reaction takes out three-neck flask from oil bath；
Step 9：After cooled to room temperature, the black suspension in bottle is filtered to remove in draught cupboard after three-neck flask
It removes to swim in apparent large stretch of carbon-coating on liquid level, redox graphene is obtained after then suspension is filtered and dried；
Step 10：Using redox graphene made from step 9 as raw material, configuration concentration is the redox graphene of 5mg/mL
Aqueous solution 40mL is placed in the plastic bottle that capacity is 60mL, the potassium hydroxide solution of point a concentration of 6mol/L of addition 3mL, abundant magnetic
Power stirs 2h and places 12h after sealing under room temperature；
Step 11：Mixed liquor made from step 10 is subjected to freeze-drying 72h at -55 DEG C；
Step 12：Sample after freeze-drying is placed in tube furnace, is heat-treated under argon gas atmosphere protection：First to pipe
Formula stove carries out vacuum pumping, and setting heating rate is 20 DEG C/min, and target temperature is 800 DEG C, soaking time 30min, argon
Throughput is 400sccm, and operating air pressure 100Pa cools to room temperature with the furnace after reaction；
Step 13：The product of step 12 is washed 2 times, then be washed with deionized with the aqueous hydrochloric acid solution that volume fraction is 10%
It is about 7 to pH value, product is freeze-dried, obtains the redox graphene of activation of potassium hydroxide.
The redox graphene of the activation of potassium hydroxide of the present invention can be applied to super capacitor.
Embodiment 3
A kind of method for the redox graphene for preparing activation of potassium hydroxide, including：
Step 1：5g graphite is weighed, 1g sodium nitrate, 2 grams of potassium nitrate and 2.3 grams of sodium bicarbonates are placed in the beaker of 1000mL, to burning
The 150mL concentrated sulfuric acids are slowly added in cup, beaker are placed in ice-water bath, magnetic agitation 1h;
Step 2：15g potassium permanganate and 2 grams of sodium permanganates are weighed, is slowly added in beaker and is stirred continuously, keep mixing in beaker
Close object temperature 30 DEG C hereinafter, beaker to be placed in room temperature later under be stirred continuously for 24 hours;
Step 3：Beaker is placed in ice-water bath, be slowly added to 300mL deionized waters and is stirred continuously, keeps mixture in beaker
Temperature is at 98 DEG C hereinafter, being then slowly added into the aqueous hydrogen peroxide solution that 30mL mass fractions are 30% and being stirred continuously;
Step 4：Mixed solution is packed into centrifuge tube, 30min is centrifuged under 8000rpm, supernatant liquid is removed, sediment is taken
Go out, wash and centrifuged 6 times with the aqueous hydrochloric acid solution that volume fraction is 10%, sediment is taken out to be placed in bag filter carry out by a definite date 3
The dialysis in week obtains graphite oxide suspension to remove salt ion and acid ion completely;
Step 5：Graphite oxide suspension is scattered in deionized water, configuration quality score is the suspension of 1mg/mL, to it
Ultrasonic disperse processing is carried out, ultrasonic time 1h centrifuges 30min and removes unstripped graphite oxide at 3,000 rpm, final to obtain
To graphene oxide aqueous dispersions；
Step 6：Using graphene oxide aqueous dispersions made from step 5, configuration concentration is the graphene oxide water of 0.3mg/mL
Dispersion liquid takes 500mL graphene oxide aqueous dispersions to be placed in three-neck flask；
Step 7：Three-neck flask is fixed on iron stand, middle port and side neck mouth with glass stopper are covered tightly, pass through opposite side
It is molten that neck mouth adds in the hydrazine that the ammonium hydroxide that 1mL mass fractions are 28wt.% and 80 μ L mass fractions are 80wt.% into three-neck flask
Then liquid also covers tightly this side port with glass stopper, and carry out abundant magnetic agitation；
Step 8：Spiral coil cooling tube is placed on the interstitial hole of three-neck flask, cooling water is opened and fills coiled pipe and keep water outlet
Flow in small thread shape, adjust the position of iron stand geometrical clamp, three-neck flask be placed in 95 DEG C of oil bath and reacts 1h,
Period keeps sufficient magnetic agitation, after completion of the reaction takes out three-neck flask from oil bath；
Step 9：After cooled to room temperature, the black suspension in bottle is filtered to remove in draught cupboard after three-neck flask
It removes to swim in apparent large stretch of carbon-coating on liquid level, redox graphene is obtained after then suspension is filtered and dried；
Step 10：Using redox graphene made from step 9 as raw material, configuration concentration is the redox graphene of 5mg/mL
Aqueous solution 40mL is placed in the plastic bottle that capacity is 60mL, the potassium hydroxide solution of point a concentration of 6mol/L of addition 3mL, abundant magnetic
Power stirs 2h and places 12h after sealing under room temperature；
Step 11：Mixed liquor made from step 10 is subjected to freeze-drying 72h at -55 DEG C；
Step 12：Sample after freeze-drying is placed in tube furnace, is heat-treated under argon gas atmosphere protection：First to pipe
Formula stove carries out vacuum pumping, and setting heating rate is 20 DEG C/min, and target temperature is 800 DEG C, soaking time 30min, argon
Throughput is 400sccm, and operating air pressure 100Pa cools to room temperature with the furnace after reaction；
Step 13：The product of step 12 is washed 2 times, then be washed with deionized with the aqueous hydrochloric acid solution that volume fraction is 10%
It is about 7 to pH value, product is freeze-dried, obtains the redox graphene of activation of potassium hydroxide.
The redox graphene of the activation of potassium hydroxide of the present invention can be applied to super capacitor.
Embodiment 4
A kind of method for the redox graphene for preparing activation of potassium hydroxide, including：
Step 1：5g graphite is weighed, 1g sodium nitrate, 2 grams of potassium nitrate and 2.4 grams of sodium bicarbonates are placed in the beaker of 1000mL, to burning
The 150mL concentrated sulfuric acids are slowly added in cup, beaker are placed in ice-water bath, magnetic agitation 1h;
Step 2：15g potassium permanganate and 2 grams of sodium permanganates are weighed, is slowly added in beaker and is stirred continuously, keep mixing in beaker
Close object temperature 30 DEG C hereinafter, beaker to be placed in room temperature later under be stirred continuously for 24 hours;
Step 3：Beaker is placed in ice-water bath, be slowly added to 300mL deionized waters and is stirred continuously, keeps mixture in beaker
Temperature is at 98 DEG C hereinafter, being then slowly added into the aqueous hydrogen peroxide solution that 30mL mass fractions are 30% and being stirred continuously;
Step 4：Mixed solution is packed into centrifuge tube, 30min is centrifuged under 8000rpm, supernatant liquid is removed, sediment is taken
Go out, wash and centrifuged 6 times with the aqueous hydrochloric acid solution that volume fraction is 10%, sediment is taken out to be placed in bag filter carry out by a definite date 3
The dialysis in week obtains graphite oxide suspension to remove salt ion and acid ion completely;
Step 5：Graphite oxide suspension is scattered in deionized water, configuration quality score is the suspension of 1mg/mL, to it
Ultrasonic disperse processing is carried out, ultrasonic time 1h centrifuges 30min and removes unstripped graphite oxide at 3,000 rpm, final to obtain
To graphene oxide aqueous dispersions；
Step 6：Using graphene oxide aqueous dispersions made from step 5, configuration concentration is the graphene oxide water of 0.3mg/mL
Dispersion liquid takes 500mL graphene oxide aqueous dispersions to be placed in three-neck flask；
Step 7：Three-neck flask is fixed on iron stand, middle port and side neck mouth with glass stopper are covered tightly, pass through opposite side
It is molten that neck mouth adds in the hydrazine that the ammonium hydroxide that 1mL mass fractions are 28wt.% and 80 μ L mass fractions are 80wt.% into three-neck flask
Then liquid also covers tightly this side port with glass stopper, and carry out abundant magnetic agitation；
Step 8：Spiral coil cooling tube is placed on the interstitial hole of three-neck flask, cooling water is opened and fills coiled pipe and keep water outlet
Flow in small thread shape, adjust the position of iron stand geometrical clamp, three-neck flask be placed in 95 DEG C of oil bath and reacts 1h,
Period keeps sufficient magnetic agitation, after completion of the reaction takes out three-neck flask from oil bath；
Step 9：After cooled to room temperature, the black suspension in bottle is filtered to remove in draught cupboard after three-neck flask
It removes to swim in apparent large stretch of carbon-coating on liquid level, redox graphene is obtained after then suspension is filtered and dried；
Step 10：Using redox graphene made from step 9 as raw material, configuration concentration is the redox graphene of 5mg/mL
Aqueous solution 40mL is placed in the plastic bottle that capacity is 60mL, the potassium hydroxide solution of point a concentration of 6mol/L of addition 3mL, abundant magnetic
Power stirs 2h and places 12h after sealing under room temperature；
Step 11：Mixed liquor made from step 10 is subjected to freeze-drying 72h at -55 DEG C；
Step 12：Sample after freeze-drying is placed in tube furnace, is heat-treated under argon gas atmosphere protection：First to pipe
Formula stove carries out vacuum pumping, and setting heating rate is 20 DEG C/min, and target temperature is 800 DEG C, soaking time 30min, argon
Throughput is 400sccm, and operating air pressure 100Pa cools to room temperature with the furnace after reaction；
Step 13：The product of step 12 is washed 2 times, then be washed with deionized with the aqueous hydrochloric acid solution that volume fraction is 10%
It is about 7 to pH value, product is freeze-dried, obtains the redox graphene of activation of potassium hydroxide.
The redox graphene of the activation of potassium hydroxide of the present invention can be applied to super capacitor.
Embodiment 5
A kind of method for the redox graphene for preparing activation of potassium hydroxide, including：
Step 1：5g graphite is weighed, 1g sodium nitrate, 2 grams of potassium nitrate and 2.5 grams of sodium bicarbonates are placed in the beaker of 1000mL, to burning
The 150mL concentrated sulfuric acids are slowly added in cup, beaker are placed in ice-water bath, magnetic agitation 1h;
Step 2：15g potassium permanganate and 2 grams of sodium permanganates are weighed, is slowly added in beaker and is stirred continuously, keep mixing in beaker
Close object temperature 30 DEG C hereinafter, beaker to be placed in room temperature later under be stirred continuously for 24 hours;
Step 3：Beaker is placed in ice-water bath, be slowly added to 300mL deionized waters and is stirred continuously, keeps mixture in beaker
Temperature is at 98 DEG C hereinafter, being then slowly added into the aqueous hydrogen peroxide solution that 30mL mass fractions are 30% and being stirred continuously;
Step 4：Mixed solution is packed into centrifuge tube, 30min is centrifuged under 8000rpm, supernatant liquid is removed, sediment is taken
Go out, wash and centrifuged 6 times with the aqueous hydrochloric acid solution that volume fraction is 10%, sediment is taken out to be placed in bag filter carry out by a definite date 3
The dialysis in week obtains graphite oxide suspension to remove salt ion and acid ion completely;
Step 5：Graphite oxide suspension is scattered in deionized water, configuration quality score is the suspension of 1mg/mL, to it
Ultrasonic disperse processing is carried out, ultrasonic time 1h centrifuges 30min and removes unstripped graphite oxide at 3,000 rpm, final to obtain
To graphene oxide aqueous dispersions；
Step 6：Using graphene oxide aqueous dispersions made from step 5, configuration concentration is the graphene oxide water of 0.3mg/mL
Dispersion liquid takes 500mL graphene oxide aqueous dispersions to be placed in three-neck flask；
Step 7：Three-neck flask is fixed on iron stand, middle port and side neck mouth with glass stopper are covered tightly, pass through opposite side
It is molten that neck mouth adds in the hydrazine that the ammonium hydroxide that 1mL mass fractions are 28wt.% and 80 μ L mass fractions are 80wt.% into three-neck flask
Then liquid also covers tightly this side port with glass stopper, and carry out abundant magnetic agitation；
Step 8：Spiral coil cooling tube is placed on the interstitial hole of three-neck flask, cooling water is opened and fills coiled pipe and keep water outlet
Flow in small thread shape, adjust the position of iron stand geometrical clamp, three-neck flask be placed in 95 DEG C of oil bath and reacts 1h,
Period keeps sufficient magnetic agitation, after completion of the reaction takes out three-neck flask from oil bath；
Step 9：After cooled to room temperature, the black suspension in bottle is filtered to remove in draught cupboard after three-neck flask
It removes to swim in apparent large stretch of carbon-coating on liquid level, redox graphene is obtained after then suspension is filtered and dried；
Step 10：Using redox graphene made from step 9 as raw material, configuration concentration is the redox graphene of 5mg/mL
Aqueous solution 40mL is placed in the plastic bottle that capacity is 60mL, the potassium hydroxide solution of point a concentration of 6mol/L of addition 3mL, abundant magnetic
Power stirs 2h and places 12h after sealing under room temperature；
Step 11：Mixed liquor made from step 10 is subjected to freeze-drying 72h at -55 DEG C；
Step 12：Sample after freeze-drying is placed in tube furnace, is heat-treated under argon gas atmosphere protection：First to pipe
Formula stove carries out vacuum pumping, and setting heating rate is 20 DEG C/min, and target temperature is 800 DEG C, soaking time 30min, argon
Throughput is 400sccm, and operating air pressure 100Pa cools to room temperature with the furnace after reaction；
Step 13：The product of step 12 is washed 2 times, then be washed with deionized with the aqueous hydrochloric acid solution that volume fraction is 10%
It is about 7 to pH value, product is freeze-dried, obtains the redox graphene of activation of potassium hydroxide.
The redox graphene of the activation of potassium hydroxide of the present invention can be applied to super capacitor.
Embodiment 6
A kind of method for the redox graphene for preparing activation of potassium hydroxide, including：
Step 1：5g graphite is weighed, 1g sodium nitrate, 2 grams of potassium nitrate and 2.6 grams of sodium bicarbonates are placed in the beaker of 1000mL, to burning
The 150mL concentrated sulfuric acids are slowly added in cup, beaker are placed in ice-water bath, magnetic agitation 1h;
Step 2：15g potassium permanganate and 2 grams of sodium permanganates are weighed, is slowly added in beaker and is stirred continuously, keep mixing in beaker
Close object temperature 30 DEG C hereinafter, beaker to be placed in room temperature later under be stirred continuously for 24 hours;
Step 3：Beaker is placed in ice-water bath, be slowly added to 300mL deionized waters and is stirred continuously, keeps mixture in beaker
Temperature is at 98 DEG C hereinafter, being then slowly added into the aqueous hydrogen peroxide solution that 30mL mass fractions are 30% and being stirred continuously;
Step 4：Mixed solution is packed into centrifuge tube, 30min is centrifuged under 8000rpm, supernatant liquid is removed, sediment is taken
Go out, wash and centrifuged 6 times with the aqueous hydrochloric acid solution that volume fraction is 10%, sediment is taken out to be placed in bag filter carry out by a definite date 3
The dialysis in week obtains graphite oxide suspension to remove salt ion and acid ion completely;
Step 5：Graphite oxide suspension is scattered in deionized water, configuration quality score is the suspension of 1mg/mL, to it
Ultrasonic disperse processing is carried out, ultrasonic time 1h centrifuges 30min and removes unstripped graphite oxide at 3,000 rpm, final to obtain
To graphene oxide aqueous dispersions；
Step 6：Using graphene oxide aqueous dispersions made from step 5, configuration concentration is the graphene oxide water of 0.3mg/mL
Dispersion liquid takes 500mL graphene oxide aqueous dispersions to be placed in three-neck flask；
Step 7：Three-neck flask is fixed on iron stand, middle port and side neck mouth with glass stopper are covered tightly, pass through opposite side
It is molten that neck mouth adds in the hydrazine that the ammonium hydroxide that 1mL mass fractions are 28wt.% and 80 μ L mass fractions are 80wt.% into three-neck flask
Then liquid also covers tightly this side port with glass stopper, and carry out abundant magnetic agitation；
Step 8：Spiral coil cooling tube is placed on the interstitial hole of three-neck flask, cooling water is opened and fills coiled pipe and keep water outlet
Flow in small thread shape, adjust the position of iron stand geometrical clamp, three-neck flask be placed in 95 DEG C of oil bath and reacts 1h,
Period keeps sufficient magnetic agitation, after completion of the reaction takes out three-neck flask from oil bath；
Step 9：After cooled to room temperature, the black suspension in bottle is filtered to remove in draught cupboard after three-neck flask
It removes to swim in apparent large stretch of carbon-coating on liquid level, redox graphene is obtained after then suspension is filtered and dried；
Step 10：Using redox graphene made from step 9 as raw material, configuration concentration is the redox graphene of 5mg/mL
Aqueous solution 40mL is placed in the plastic bottle that capacity is 60mL, the potassium hydroxide solution of point a concentration of 6mol/L of addition 3mL, abundant magnetic
Power stirs 2h and places 12h after sealing under room temperature；
Step 11：Mixed liquor made from step 10 is subjected to freeze-drying 72h at -55 DEG C；
Step 12：Sample after freeze-drying is placed in tube furnace, is heat-treated under argon gas atmosphere protection：First to pipe
Formula stove carries out vacuum pumping, and setting heating rate is 20 DEG C/min, and target temperature is 800 DEG C, soaking time 30min, argon
Throughput is 400sccm, and operating air pressure 100Pa cools to room temperature with the furnace after reaction；
Step 13：The product of step 12 is washed 2 times, then be washed with deionized with the aqueous hydrochloric acid solution that volume fraction is 10%
It is about 7 to pH value, product is freeze-dried, obtains the redox graphene of activation of potassium hydroxide.
The redox graphene of the activation of potassium hydroxide of the present invention can be applied to super capacitor.
Embodiment 7
A kind of method for the redox graphene for preparing activation of potassium hydroxide, including：
Step 1：5g graphite is weighed, 1g sodium nitrate, 2 grams of potassium nitrate and 2.7 grams of sodium bicarbonates are placed in the beaker of 1000mL, to burning
The 150mL concentrated sulfuric acids are slowly added in cup, beaker are placed in ice-water bath, magnetic agitation 1h;
Step 2：15g potassium permanganate and 2 grams of sodium permanganates are weighed, is slowly added in beaker and is stirred continuously, keep mixing in beaker
Close object temperature 30 DEG C hereinafter, beaker to be placed in room temperature later under be stirred continuously for 24 hours;
Step 3：Beaker is placed in ice-water bath, be slowly added to 300mL deionized waters and is stirred continuously, keeps mixture in beaker
Temperature is at 98 DEG C hereinafter, being then slowly added into the aqueous hydrogen peroxide solution that 30mL mass fractions are 30% and being stirred continuously;
Step 4：Mixed solution is packed into centrifuge tube, 30min is centrifuged under 8000rpm, supernatant liquid is removed, sediment is taken
Go out, wash and centrifuged 6 times with the aqueous hydrochloric acid solution that volume fraction is 10%, sediment is taken out to be placed in bag filter carry out by a definite date 3
The dialysis in week obtains graphite oxide suspension to remove salt ion and acid ion completely;
Step 5：Graphite oxide suspension is scattered in deionized water, configuration quality score is the suspension of 1mg/mL, to it
Ultrasonic disperse processing is carried out, ultrasonic time 1h centrifuges 30min and removes unstripped graphite oxide at 3,000 rpm, final to obtain
To graphene oxide aqueous dispersions；
Step 6：Using graphene oxide aqueous dispersions made from step 5, configuration concentration is the graphene oxide water of 0.3mg/mL
Dispersion liquid takes 500mL graphene oxide aqueous dispersions to be placed in three-neck flask；
Step 7：Three-neck flask is fixed on iron stand, middle port and side neck mouth with glass stopper are covered tightly, pass through opposite side
It is molten that neck mouth adds in the hydrazine that the ammonium hydroxide that 1mL mass fractions are 28wt.% and 80 μ L mass fractions are 80wt.% into three-neck flask
Then liquid also covers tightly this side port with glass stopper, and carry out abundant magnetic agitation；
Step 8：Spiral coil cooling tube is placed on the interstitial hole of three-neck flask, cooling water is opened and fills coiled pipe and keep water outlet
Flow in small thread shape, adjust the position of iron stand geometrical clamp, three-neck flask be placed in 95 DEG C of oil bath and reacts 1h,
Period keeps sufficient magnetic agitation, after completion of the reaction takes out three-neck flask from oil bath；
Step 9：After cooled to room temperature, the black suspension in bottle is filtered to remove in draught cupboard after three-neck flask
It removes to swim in apparent large stretch of carbon-coating on liquid level, redox graphene is obtained after then suspension is filtered and dried；
Step 10：Using redox graphene made from step 9 as raw material, configuration concentration is the redox graphene of 5mg/mL
Aqueous solution 40mL is placed in the plastic bottle that capacity is 60mL, the potassium hydroxide solution of point a concentration of 6mol/L of addition 3mL, abundant magnetic
Power stirs 2h and places 12h after sealing under room temperature；
Step 11：Mixed liquor made from step 10 is subjected to freeze-drying 72h at -55 DEG C；
Step 12：Sample after freeze-drying is placed in tube furnace, is heat-treated under argon gas atmosphere protection：First to pipe
Formula stove carries out vacuum pumping, and setting heating rate is 20 DEG C/min, and target temperature is 800 DEG C, soaking time 30min, argon
Throughput is 400sccm, and operating air pressure 100Pa cools to room temperature with the furnace after reaction；
Step 13：The product of step 12 is washed 2 times, then be washed with deionized with the aqueous hydrochloric acid solution that volume fraction is 10%
It is about 7 to pH value, product is freeze-dried, obtains the redox graphene of activation of potassium hydroxide.
The redox graphene of the activation of potassium hydroxide of the present invention can be applied to super capacitor.
Embodiment 8
A kind of method for the redox graphene for preparing activation of potassium hydroxide, including：
Step 1：5g graphite is weighed, 1g sodium nitrate, 2 grams of potassium nitrate and 2.8 grams of sodium bicarbonates are placed in the beaker of 1000mL, to burning
The 150mL concentrated sulfuric acids are slowly added in cup, beaker are placed in ice-water bath, magnetic agitation 1h;
Step 2：15g potassium permanganate and 2 grams of sodium permanganates are weighed, is slowly added in beaker and is stirred continuously, keep mixing in beaker
Close object temperature 30 DEG C hereinafter, beaker to be placed in room temperature later under be stirred continuously for 24 hours;
Step 3：Beaker is placed in ice-water bath, be slowly added to 300mL deionized waters and is stirred continuously, keeps mixture in beaker
Temperature is at 98 DEG C hereinafter, being then slowly added into the aqueous hydrogen peroxide solution that 30mL mass fractions are 30% and being stirred continuously;
Step 4：Mixed solution is packed into centrifuge tube, 30min is centrifuged under 8000rpm, supernatant liquid is removed, sediment is taken
Go out, wash and centrifuged 6 times with the aqueous hydrochloric acid solution that volume fraction is 10%, sediment is taken out to be placed in bag filter carry out by a definite date 3
The dialysis in week obtains graphite oxide suspension to remove salt ion and acid ion completely;
Step 5：Graphite oxide suspension is scattered in deionized water, configuration quality score is the suspension of 1mg/mL, to it
Ultrasonic disperse processing is carried out, ultrasonic time 1h centrifuges 30min and removes unstripped graphite oxide at 3,000 rpm, final to obtain
To graphene oxide aqueous dispersions；
Step 6：Using graphene oxide aqueous dispersions made from step 5, configuration concentration is the graphene oxide water of 0.3mg/mL
Dispersion liquid takes 500mL graphene oxide aqueous dispersions to be placed in three-neck flask；
Step 7：Three-neck flask is fixed on iron stand, middle port and side neck mouth with glass stopper are covered tightly, pass through opposite side
It is molten that neck mouth adds in the hydrazine that the ammonium hydroxide that 1mL mass fractions are 28wt.% and 80 μ L mass fractions are 80wt.% into three-neck flask
Then liquid also covers tightly this side port with glass stopper, and carry out abundant magnetic agitation；
Step 8：Spiral coil cooling tube is placed on the interstitial hole of three-neck flask, cooling water is opened and fills coiled pipe and keep water outlet
Flow in small thread shape, adjust the position of iron stand geometrical clamp, three-neck flask be placed in 95 DEG C of oil bath and reacts 1h,
Period keeps sufficient magnetic agitation, after completion of the reaction takes out three-neck flask from oil bath；
Step 9：After cooled to room temperature, the black suspension in bottle is filtered to remove in draught cupboard after three-neck flask
It removes to swim in apparent large stretch of carbon-coating on liquid level, redox graphene is obtained after then suspension is filtered and dried；
Step 10：Using redox graphene made from step 9 as raw material, configuration concentration is the redox graphene of 5mg/mL
Aqueous solution 40mL is placed in the plastic bottle that capacity is 60mL, the potassium hydroxide solution of point a concentration of 6mol/L of addition 3mL, abundant magnetic
Power stirs 2h and places 12h after sealing under room temperature；
Step 11：Mixed liquor made from step 10 is subjected to freeze-drying 72h at -55 DEG C；
Step 12：Sample after freeze-drying is placed in tube furnace, is heat-treated under argon gas atmosphere protection：First to pipe
Formula stove carries out vacuum pumping, and setting heating rate is 20 DEG C/min, and target temperature is 800 DEG C, soaking time 30min, argon
Throughput is 400sccm, and operating air pressure 100Pa cools to room temperature with the furnace after reaction；
Step 13：The product of step 12 is washed 2 times, then be washed with deionized with the aqueous hydrochloric acid solution that volume fraction is 10%
It is about 7 to pH value, product is freeze-dried, obtains the redox graphene of activation of potassium hydroxide.
The redox graphene of the activation of potassium hydroxide of the present invention can be applied to super capacitor.
Embodiment 9
A kind of method for the redox graphene for preparing activation of potassium hydroxide, including：
Step 1：5g graphite is weighed, 1g sodium nitrate, 2 grams of potassium nitrate and 2.9 grams of sodium bicarbonates are placed in the beaker of 1000mL, to burning
The 150mL concentrated sulfuric acids are slowly added in cup, beaker are placed in ice-water bath, magnetic agitation 1h;
Step 2：15g potassium permanganate and 2 grams of sodium permanganates are weighed, is slowly added in beaker and is stirred continuously, keep mixing in beaker
Close object temperature 30 DEG C hereinafter, beaker to be placed in room temperature later under be stirred continuously for 24 hours;
Step 3：Beaker is placed in ice-water bath, be slowly added to 300mL deionized waters and is stirred continuously, keeps mixture in beaker
Temperature is at 98 DEG C hereinafter, being then slowly added into the aqueous hydrogen peroxide solution that 30mL mass fractions are 30% and being stirred continuously;
Step 4：Mixed solution is packed into centrifuge tube, 30min is centrifuged under 8000rpm, supernatant liquid is removed, sediment is taken
Go out, wash and centrifuged 6 times with the aqueous hydrochloric acid solution that volume fraction is 10%, sediment is taken out to be placed in bag filter carry out by a definite date 3
The dialysis in week obtains graphite oxide suspension to remove salt ion and acid ion completely;
Step 5：Graphite oxide suspension is scattered in deionized water, configuration quality score is the suspension of 1mg/mL, to it
Ultrasonic disperse processing is carried out, ultrasonic time 1h centrifuges 30min and removes unstripped graphite oxide at 3,000 rpm, final to obtain
To graphene oxide aqueous dispersions；
Step 6：Using graphene oxide aqueous dispersions made from step 5, configuration concentration is the graphene oxide water of 0.3mg/mL
Dispersion liquid takes 500mL graphene oxide aqueous dispersions to be placed in three-neck flask；
Step 7：Three-neck flask is fixed on iron stand, middle port and side neck mouth with glass stopper are covered tightly, pass through opposite side
It is molten that neck mouth adds in the hydrazine that the ammonium hydroxide that 1mL mass fractions are 28wt.% and 80 μ L mass fractions are 80wt.% into three-neck flask
Then liquid also covers tightly this side port with glass stopper, and carry out abundant magnetic agitation；
Step 8：Spiral coil cooling tube is placed on the interstitial hole of three-neck flask, cooling water is opened and fills coiled pipe and keep water outlet
Flow in small thread shape, adjust the position of iron stand geometrical clamp, three-neck flask be placed in 95 DEG C of oil bath and reacts 1h,
Period keeps sufficient magnetic agitation, after completion of the reaction takes out three-neck flask from oil bath；
Step 9：After cooled to room temperature, the black suspension in bottle is filtered to remove in draught cupboard after three-neck flask
It removes to swim in apparent large stretch of carbon-coating on liquid level, redox graphene is obtained after then suspension is filtered and dried；
Step 10：Using redox graphene made from step 9 as raw material, configuration concentration is the redox graphene of 5mg/mL
Aqueous solution 40mL is placed in the plastic bottle that capacity is 60mL, the potassium hydroxide solution of point a concentration of 6mol/L of addition 3mL, abundant magnetic
Power stirs 2h and places 12h after sealing under room temperature；
Step 11：Mixed liquor made from step 10 is subjected to freeze-drying 72h at -55 DEG C；
Step 12：Sample after freeze-drying is placed in tube furnace, is heat-treated under argon gas atmosphere protection：First to pipe
Formula stove carries out vacuum pumping, and setting heating rate is 20 DEG C/min, and target temperature is 800 DEG C, soaking time 30min, argon
Throughput is 400sccm, and operating air pressure 100Pa cools to room temperature with the furnace after reaction；
Step 13：The product of step 12 is washed 2 times, then be washed with deionized with the aqueous hydrochloric acid solution that volume fraction is 10%
It is about 7 to pH value, product is freeze-dried, obtains the redox graphene of activation of potassium hydroxide.
The redox graphene of the activation of potassium hydroxide of the present invention can be applied to super capacitor.
Embodiment 10
A kind of method for the redox graphene for preparing activation of potassium hydroxide, including：
Step 1：5g graphite is weighed, 1g sodium nitrate, 2 grams of potassium nitrate and 3 grams of sodium bicarbonates are placed in the beaker of 1000mL, to beaker
In be slowly added to the 150mL concentrated sulfuric acids, beaker is placed in ice-water bath, magnetic agitation 1h;
Step 2：15g potassium permanganate and 2 grams of sodium permanganates are weighed, is slowly added in beaker and is stirred continuously, keep mixing in beaker
Close object temperature 30 DEG C hereinafter, beaker to be placed in room temperature later under be stirred continuously for 24 hours;
Step 3：Beaker is placed in ice-water bath, be slowly added to 300mL deionized waters and is stirred continuously, keeps mixture in beaker
Temperature is at 98 DEG C hereinafter, being then slowly added into the aqueous hydrogen peroxide solution that 30mL mass fractions are 30% and being stirred continuously;
Step 4：Mixed solution is packed into centrifuge tube, 30min is centrifuged under 8000rpm, supernatant liquid is removed, sediment is taken
Go out, wash and centrifuged 6 times with the aqueous hydrochloric acid solution that volume fraction is 10%, sediment is taken out to be placed in bag filter carry out by a definite date 3
The dialysis in week obtains graphite oxide suspension to remove salt ion and acid ion completely;
Step 5：Graphite oxide suspension is scattered in deionized water, configuration quality score is the suspension of 1mg/mL, to it
Ultrasonic disperse processing is carried out, ultrasonic time 1h centrifuges 30min and removes unstripped graphite oxide at 3,000 rpm, final to obtain
To graphene oxide aqueous dispersions；
Step 6：Using graphene oxide aqueous dispersions made from step 5, configuration concentration is the graphene oxide water of 0.3mg/mL
Dispersion liquid takes 500mL graphene oxide aqueous dispersions to be placed in three-neck flask；
Step 7：Three-neck flask is fixed on iron stand, middle port and side neck mouth with glass stopper are covered tightly, pass through opposite side
It is molten that neck mouth adds in the hydrazine that the ammonium hydroxide that 1mL mass fractions are 28wt.% and 80 μ L mass fractions are 80wt.% into three-neck flask
Then liquid also covers tightly this side port with glass stopper, and carry out abundant magnetic agitation；
Step 8：Spiral coil cooling tube is placed on the interstitial hole of three-neck flask, cooling water is opened and fills coiled pipe and keep water outlet
Flow in small thread shape, adjust the position of iron stand geometrical clamp, three-neck flask be placed in 95 DEG C of oil bath and reacts 1h,
Period keeps sufficient magnetic agitation, after completion of the reaction takes out three-neck flask from oil bath；
Step 9：After cooled to room temperature, the black suspension in bottle is filtered to remove in draught cupboard after three-neck flask
It removes to swim in apparent large stretch of carbon-coating on liquid level, redox graphene is obtained after then suspension is filtered and dried；
Step 10：Using redox graphene made from step 9 as raw material, configuration concentration is the redox graphene of 5mg/mL
Aqueous solution 40mL is placed in the plastic bottle that capacity is 60mL, the potassium hydroxide solution of point a concentration of 6mol/L of addition 3mL, abundant magnetic
Power stirs 2h and places 12h after sealing under room temperature；
Step 11：Mixed liquor made from step 10 is subjected to freeze-drying 72h at -55 DEG C；
Step 12：Sample after freeze-drying is placed in tube furnace, is heat-treated under argon gas atmosphere protection：First to pipe
Formula stove carries out vacuum pumping, and setting heating rate is 20 DEG C/min, and target temperature is 800 DEG C, soaking time 30min, argon
Throughput is 400sccm, and operating air pressure 100Pa cools to room temperature with the furnace after reaction；
Step 13：The product of step 12 is washed 2 times, then be washed with deionized with the aqueous hydrochloric acid solution that volume fraction is 10%
It is about 7 to pH value, product is freeze-dried, obtains the redox graphene of activation of potassium hydroxide.
The redox graphene of the activation of potassium hydroxide of the present invention can be applied to super capacitor.
Embodiment 11
A kind of method for the redox graphene for preparing activation of potassium hydroxide, including：
Step 1：5g graphite is weighed, 1g sodium nitrate, 2 grams of potassium nitrate and 3.1 grams of sodium bicarbonates are placed in the beaker of 1000mL, to burning
The 150mL concentrated sulfuric acids are slowly added in cup, beaker are placed in ice-water bath, magnetic agitation 1h;
Step 2：15g potassium permanganate and 2 grams of sodium permanganates are weighed, is slowly added in beaker and is stirred continuously, keep mixing in beaker
Close object temperature 30 DEG C hereinafter, beaker to be placed in room temperature later under be stirred continuously for 24 hours;
Step 3：Beaker is placed in ice-water bath, be slowly added to 300mL deionized waters and is stirred continuously, keeps mixture in beaker
Temperature is at 98 DEG C hereinafter, being then slowly added into the aqueous hydrogen peroxide solution that 30mL mass fractions are 30% and being stirred continuously;
Step 4：Mixed solution is packed into centrifuge tube, 30min is centrifuged under 8000rpm, supernatant liquid is removed, sediment is taken
Go out, wash and centrifuged 6 times with the aqueous hydrochloric acid solution that volume fraction is 10%, sediment is taken out to be placed in bag filter carry out by a definite date 3
The dialysis in week obtains graphite oxide suspension to remove salt ion and acid ion completely;
Step 5：Graphite oxide suspension is scattered in deionized water, configuration quality score is the suspension of 1mg/mL, to it
Ultrasonic disperse processing is carried out, ultrasonic time 1h centrifuges 30min and removes unstripped graphite oxide at 3,000 rpm, final to obtain
To graphene oxide aqueous dispersions；
Step 6：Using graphene oxide aqueous dispersions made from step 5, configuration concentration is the graphene oxide water of 0.3mg/mL
Dispersion liquid takes 500mL graphene oxide aqueous dispersions to be placed in three-neck flask；
Step 7：Three-neck flask is fixed on iron stand, middle port and side neck mouth with glass stopper are covered tightly, pass through opposite side
It is molten that neck mouth adds in the hydrazine that the ammonium hydroxide that 1mL mass fractions are 28wt.% and 80 μ L mass fractions are 80wt.% into three-neck flask
Then liquid also covers tightly this side port with glass stopper, and carry out abundant magnetic agitation；
Step 8：Spiral coil cooling tube is placed on the interstitial hole of three-neck flask, cooling water is opened and fills coiled pipe and keep water outlet
Flow in small thread shape, adjust the position of iron stand geometrical clamp, three-neck flask be placed in 95 DEG C of oil bath and reacts 1h,
Period keeps sufficient magnetic agitation, after completion of the reaction takes out three-neck flask from oil bath；
Step 9：After cooled to room temperature, the black suspension in bottle is filtered to remove in draught cupboard after three-neck flask
It removes to swim in apparent large stretch of carbon-coating on liquid level, redox graphene is obtained after then suspension is filtered and dried；
Step 10：Using redox graphene made from step 9 as raw material, configuration concentration is the redox graphene of 5mg/mL
Aqueous solution 40mL is placed in the plastic bottle that capacity is 60mL, the potassium hydroxide solution of point a concentration of 6mol/L of addition 3mL, abundant magnetic
Power stirs 2h and places 12h after sealing under room temperature；
Step 11：Mixed liquor made from step 10 is subjected to freeze-drying 72h at -55 DEG C；
Step 12：Sample after freeze-drying is placed in tube furnace, is heat-treated under argon gas atmosphere protection：First to pipe
Formula stove carries out vacuum pumping, and setting heating rate is 20 DEG C/min, and target temperature is 800 DEG C, soaking time 30min, argon
Throughput is 400sccm, and operating air pressure 100Pa cools to room temperature with the furnace after reaction；
Step 13：The product of step 12 is washed 2 times, then be washed with deionized with the aqueous hydrochloric acid solution that volume fraction is 10%
It is about 7 to pH value, product is freeze-dried, obtains the redox graphene of activation of potassium hydroxide.
The redox graphene of the activation of potassium hydroxide of the present invention can be applied to super capacitor.
Claims (2)
1. a kind of method for the redox graphene for preparing activation of potassium hydroxide, including：
Step 1：5g graphite is weighed, 1g sodium nitrate, 2 grams of potassium nitrate and 2 grams of sodium bicarbonates are placed in the beaker of 1000mL, to beaker
In be slowly added to the 150mL concentrated sulfuric acids, beaker is placed in ice-water bath, magnetic agitation 1h;
Step 2：15g potassium permanganate and 2 grams of sodium permanganates are weighed, is slowly added in beaker and is stirred continuously, keep mixing in beaker
Close object temperature 30 DEG C hereinafter, beaker to be placed in room temperature later under be stirred continuously for 24 hours;
Step 3：Beaker is placed in ice-water bath, be slowly added to 300mL deionized waters and is stirred continuously, keeps mixture in beaker
Temperature is at 98 DEG C hereinafter, being then slowly added into the aqueous hydrogen peroxide solution that 30mL mass fractions are 30% and being stirred continuously;
Step 4：Mixed solution is packed into centrifuge tube, 30min is centrifuged under 8000rpm, supernatant liquid is removed, sediment is taken
Go out, wash and centrifuged 6 times with the aqueous hydrochloric acid solution that volume fraction is 10%, sediment is taken out to be placed in bag filter carry out by a definite date 3
The dialysis in week obtains graphite oxide suspension to remove salt ion and acid ion completely;
Step 5：Graphite oxide suspension is scattered in deionized water, configuration quality score is the suspension of 1mg/mL, to it
Ultrasonic disperse processing is carried out, ultrasonic time 1h centrifuges 30min and removes unstripped graphite oxide at 3,000 rpm, final to obtain
To graphene oxide aqueous dispersions；
Step 6：Using graphene oxide aqueous dispersions made from step 5, configuration concentration is the graphene oxide water of 0.3mg/mL
Dispersion liquid takes 500mL graphene oxide aqueous dispersions to be placed in three-neck flask；
Step 7：Three-neck flask is fixed on iron stand, middle port and side neck mouth with glass stopper are covered tightly, pass through opposite side
It is molten that neck mouth adds in the hydrazine that the ammonium hydroxide that 1mL mass fractions are 28wt.% and 80 μ L mass fractions are 80wt.% into three-neck flask
Then liquid also covers tightly this side port with glass stopper, and carry out abundant magnetic agitation；
Step 8：Spiral coil cooling tube is placed on the interstitial hole of three-neck flask, cooling water is opened and fills coiled pipe and keep water outlet
Flow in small thread shape, adjust the position of iron stand geometrical clamp, three-neck flask be placed in 95 DEG C of oil bath and reacts 1h,
Period keeps sufficient magnetic agitation, after completion of the reaction takes out three-neck flask from oil bath；
Step 9：After cooled to room temperature, the black suspension in bottle is filtered to remove in draught cupboard after three-neck flask
It removes to swim in apparent large stretch of carbon-coating on liquid level, redox graphene is obtained after then suspension is filtered and dried；
Step 10：Using redox graphene made from step 9 as raw material, configuration concentration is the redox graphene of 5mg/mL
Aqueous solution 40mL is placed in the plastic bottle that capacity is 60mL, the potassium hydroxide solution of point a concentration of 6mol/L of addition 3mL, abundant magnetic
Power stirs 2h and places 12h after sealing under room temperature；
Step 11：Mixed liquor made from step 10 is subjected to freeze-drying 72h at -55 DEG C；
Step 12：Sample after freeze-drying is placed in tube furnace, is heat-treated under argon gas atmosphere protection：First to pipe
Formula stove carries out vacuum pumping, and setting heating rate is 20 DEG C/min, and target temperature is 800 DEG C, soaking time 30min, argon
Throughput is 400sccm, and operating air pressure 100Pa cools to room temperature with the furnace after reaction；
Step 13：The product of step 12 is washed 2 times, then be washed with deionized with the aqueous hydrochloric acid solution that volume fraction is 10%
It is about 7 to pH value, product is freeze-dried, obtains the redox graphene of activation of potassium hydroxide.
2. the redox graphene of the activation of potassium hydroxide of the present invention can be applied to super capacitor.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108640106A (en) * | 2018-07-10 | 2018-10-12 | 杭州高烯科技有限公司 | A kind of stripping means of graphene film |
| CN112971205A (en) * | 2021-04-26 | 2021-06-18 | 昆明理工大学 | Application of graphene adsorption material in reducing harmful components in cigarette smoke |
| CN114899374A (en) * | 2022-05-07 | 2022-08-12 | 桂林理工大学 | Graphene oxide/sulfur/sisal fiber activated carbon lithium-sulfur battery composite positive electrode material and preparation method thereof |
-
2018
- 2018-04-08 CN CN201810308387.5A patent/CN108217638A/en not_active Withdrawn
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108640106A (en) * | 2018-07-10 | 2018-10-12 | 杭州高烯科技有限公司 | A kind of stripping means of graphene film |
| CN112971205A (en) * | 2021-04-26 | 2021-06-18 | 昆明理工大学 | Application of graphene adsorption material in reducing harmful components in cigarette smoke |
| CN114899374A (en) * | 2022-05-07 | 2022-08-12 | 桂林理工大学 | Graphene oxide/sulfur/sisal fiber activated carbon lithium-sulfur battery composite positive electrode material and preparation method thereof |
| CN114899374B (en) * | 2022-05-07 | 2023-09-22 | 桂林理工大学 | Composite positive electrode material of lithium-sulfur battery and preparation method thereof |
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