Large-scale preparation method for graphene quantum dots | Matter42 Literature
Patent
Atlas literature
Patent
US 9,663,370
Large-scale preparation method for graphene quantum dots
Mingdong ZHANG
US
Drawings
Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 3
Figure 3 is the fluorescence spectra of graphen e quantum do ts obtained f rom Embo dim ent 2; Fig u re 4 is the fluorescence spectr a of graphene quant um d ots obta i ned from Embodiment 3;
Figure 5
Figure 5 is the fluorescence spectra of gr aphene quantum dot s obtained fr om Embodiment 4. 5 Em bodi m ents To mak e the inven tion clear a nd easy to un derstand, the detailed description for specific exec u tio n m ode of this invention was accomplished combined with the figure. The concrete detai …
Figure 1
Figure 1, in one e m bodi m ent t he nieth od fo r preparing grap h ene quantum d ots in large-scale inc lu des the steps of S 110 step S 140. Step S i 10: adding g raphene oxide to a first solvent and dispersing u nifor m ly to obtain a first dispersion liquid, followed by adding a reducing agent to …
Claims
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
7 independent · 7 dependent
1
Independentgraphene oxidereducing agentreducing polyhydroxy aldehyde or organic acidLewis acid
(Currently Amended) A m eth o d for preparing graphene qua ntum dots [[in]] on a lar ge-scale, the method comprising: dispersi n g graphene oxide un i for m ly in the a first solvent to o btain a fi r st dispersion liquid, adding a reducing agent in to the fi r st dispersion liquid an d dispersing uniformly to give generate a m ixed solution: treating the mixed solution for 1 0- ~60miins u nder ai mic rowa v e en v ironment w ith ahe. power bking at of 500-8 00W, then cool in g and separating t o obtai n th z: a sol i d ac c crude produ ct; mixing onc c f the a reduci n g polyhydroxy aldehyde or an or g anic acid with the solid crude product, following by addin g the a Lewis acid to obtain a mixture, dispers ing the m ixture in a second solvent unifor m ly to obtain a second dispersion liquid; treating putting wherein the second dispersion liquid into with microwaves microwave treatment f r 0.2 -1 hours with tho a microwave p ow er bing of 500- 800 w, then stripping for ?-3 hours un der an u ltrasonic power of 120- 300w, and p urify ing to obtain thc g raphic graphene quantum dots.
2
Dependent← claim 1
2. (Currently Am ended) The method of claim 1, w herei n before the stcp treating tho mixed solution under microwave environment for 10-60mins with the microwave power being 500-800W, i ncludin g a step of ultrasonic stirring, wherein the step of ultrasonic stirring compriing: stirring the mix o d clution under n ltra s oni z ibr 0. 5 1 hours with the ultrasonic power being 120-300W a step of ultrasonic stirring is performed before the step of treating the mixed solution under the microwave environment for 10-60 mins with the microwave power of 500-800W, wherein the step of ultrasonic stirring comprises: stirring the mixed solution with the ultrasonic power of 120-300W for 0.5-4 hours.
4
Dependent← claim 1solvent
The m eth o d of claim 1, wherein the first solvent and the second solvent both c om prises at least one agent selected from the group consisting of water, di m ethoxyethane, an aqueous sol u tion of poly v inyl alcohol, glycerol a lc ohol, po lyhydrox y aldehyde and N- m ethylpy rrolidone.
6
Dependent← claim 1reducing agent
The method of claim 1, wherein the reducing agent comprises at lea s t one agent selected from the group consisting of citric acid, gluco n ic acid, fo rmic acid, ascorb i c acid. oxalic acid, sodi um citrate, so dium gh conate, sodium fo n nate, sodi mn oxalate and sodiu m ascorbate.
8
Dependent← claim 1
The method of claim 1, wherein the step of treating the mixed so lu tion for 10 -60min s under the microwave enviro nment with the microwave pow er being of 500-800 W further comprises comprising: reacting the mixed solution for 5-30mins under the microwave enviro mn ent with the microwa ve power being f 500-800W, then remov ing and Page 3 of 9 A pplic ation Serial Na.:.1/109, 8!7 Fir st Nam ed in ventor: Mingdong ZH ANG SVG 15109817.03-23-2017.J₀SFMV₂EPXXIFW2.CLM.3.svg 0.52 6.32 Black and white the microwave power being of 500--SOfAW: wherei n the a volume of the an add iti onal first solvent is 10%--15 % of a n 4re initi al vo lu e of the first solvent.
11
Dependent← claim 1Lewis acid
(O rig in al) The method of claim 1, wherein the Lewis acid comprises at least one agent selected fr om the group c o nsisti ng of fe rrie chloride, aluminru chloride, zinc chloride, boron trif lu oride, magnesi um chloride, copper chloride and lit hium chl o ride.
12
Dependent← claim 1organic acid
12. (Original) Th e method of claim 1, wherein the organi c acid comprises at least o ne agent selected f rom the group consisting of citric acid gl u conic acid formic acid, ascorbic acid and oxali e acid.
13
Dependent← claim 1Lewis acid
The method of claim 1, w herein in the. sccond dispersion liquid, the a concentration of the m ixt ur e consisting of the solid crude product, the Lewis acid and one of the reducing polyhydroxy aldehyde and the organic acid is 0. f- 1 g/ml.
5
Independentgraphene oxide
The method of c laim 1, wherein the a concentration of y raphemz graphene oxide in the first dispersion liqu id is 2~ 10 mg/nil.
7
Independentgraphene oxidereducing agent
7. (Curren t ly Amended) The m ethod of cla im I wh erein the a weight ratio of the gra ph ene oxide to the reducing ag ent is 1:3- 10.
9
Independentreducing polyhydroxy aldehyde or organic acid
(C u rre n tly Amended) The method of clai m 1, w herein t he a wei g ht ratio of the solid crude product to one of the reducing p olyhydroxy aldeh y de er and organic acid is 1:5 -40,
10
Independentreducing polyhydroxy aldehyde or organic acid
1 0. The method of clai m 1, wherein the red ucing pol yhydroxy aldehyde is glucose or adipaldehyde.
14
IndependentLewis acid
(C rren tly Amended) The method of clai 1, wherein thc a weight of the Lewis acid is 1%--3 % by weigh t of the mixture.
15
Independentgraphene quantum dots
1 5. (Currently Amen ded) The method of clai m 1, w her ein the step of obtain in g the graphene quantum dots after an isolation and a p ur ification frther comprises comprising: treatin g 4 a resultant obtained by stripping for 2 -- 3ho u rs under ultra s onic condition at 120 300W wit h column chromatog rap hy, and ev a porating u nder vac uum rotary evaporation to gi g e generate the purified graphene quantum dots; Page 4 of 9 App lication Serial No.: 15109,87 First Nam ed in vento r: Mingdong ZHJANG Art Unit: 173 6 Res ponse to OQfic e Action;nailed on 01 17/2017 wherein the a sta ti onar y phase of the chromatograp hy colunm is silica gel or pol yac ryla mide. wherein the first developin g solvent consists of is the a m ixed solution of dich lorideni ethane an d m ethanol w ith Pt e a vo lnn e r a tio being of 1:1 -3, and the second developing so l vent is-c onsists of de io nized water. Page 5 of 9
Materials
Materials described outside the worked examples.
graphene oxide
Precursor/Starting Material
reducing agent
Reducing Agent
Process steps
Additional fabrication and treatment steps described in the patent.
1
Microwave Solvothermal
Step 1
Duration
10, 60 min
Process details
purification:
Reported properties
Performance values and ranges asserted in the specification or claims.
Property
Value
Material
Duration
0.2–1 hours
—
—
Patent
Atlas literature
Patent
US 9,663,370
Large-scale preparation method for graphene quantum dots
Mingdong ZHANG
US
Drawings
Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 3
Figure 3 is the fluorescence spectra of graphen e quantum do ts obtained f rom Embo dim ent 2; Fig u re 4 is the fluorescence spectr a of graphene quant um d ots obta i ned from Embodiment 3;
Figure 5
Figure 5 is the fluorescence spectra of gr aphene quantum dot s obtained fr om Embodiment 4. 5 Em bodi m ents To mak e the inven tion clear a nd easy to un derstand, the detailed description for specific exec u tio n m ode of this invention was accomplished combined with the figure. The concrete detai …
Figure 1
Figure 1, in one e m bodi m ent t he nieth od fo r preparing grap h ene quantum d ots in large-scale inc lu des the steps of S 110 step S 140. Step S i 10: adding g raphene oxide to a first solvent and dispersing u nifor m ly to obtain a first dispersion liquid, followed by adding a reducing agent to …
Claims
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
7 independent · 7 dependent
1
Independentgraphene oxidereducing agentreducing polyhydroxy aldehyde or organic acidLewis acid
(Currently Amended) A m eth o d for preparing graphene qua ntum dots [[in]] on a lar ge-scale, the method comprising: dispersi n g graphene oxide un i for m ly in the a first solvent to o btain a fi r st dispersion liquid, adding a reducing agent in to the fi r st dispersion liquid an d dispersing uniformly to give generate a m ixed solution: treating the mixed solution for 1 0- ~60miins u nder ai mic rowa v e en v ironment w ith ahe. power bking at of 500-8 00W, then cool in g and separating t o obtai n th z: a sol i d ac c crude produ ct; mixing onc c f the a reduci n g polyhydroxy aldehyde or an or g anic acid with the solid crude product, following by addin g the a Lewis acid to obtain a mixture, dispers ing the m ixture in a second solvent unifor m ly to obtain a second dispersion liquid; treating putting wherein the second dispersion liquid into with microwaves microwave treatment f r 0.2 -1 hours with tho a microwave p ow er bing of 500- 800 w, then stripping for ?-3 hours un der an u ltrasonic power of 120- 300w, and p urify ing to obtain thc g raphic graphene quantum dots.
2
Dependent← claim 1
2. (Currently Am ended) The method of claim 1, w herei n before the stcp treating tho mixed solution under microwave environment for 10-60mins with the microwave power being 500-800W, i ncludin g a step of ultrasonic stirring, wherein the step of ultrasonic stirring compriing: stirring the mix o d clution under n ltra s oni z ibr 0. 5 1 hours with the ultrasonic power being 120-300W a step of ultrasonic stirring is performed before the step of treating the mixed solution under the microwave environment for 10-60 mins with the microwave power of 500-800W, wherein the step of ultrasonic stirring comprises: stirring the mixed solution with the ultrasonic power of 120-300W for 0.5-4 hours.
4
Dependent← claim 1solvent
The m eth o d of claim 1, wherein the first solvent and the second solvent both c om prises at least one agent selected from the group consisting of water, di m ethoxyethane, an aqueous sol u tion of poly v inyl alcohol, glycerol a lc ohol, po lyhydrox y aldehyde and N- m ethylpy rrolidone.
6
Dependent← claim 1reducing agent
The method of claim 1, wherein the reducing agent comprises at lea s t one agent selected from the group consisting of citric acid, gluco n ic acid, fo rmic acid, ascorb i c acid. oxalic acid, sodi um citrate, so dium gh conate, sodium fo n nate, sodi mn oxalate and sodiu m ascorbate.
8
Dependent← claim 1
The method of claim 1, wherein the step of treating the mixed so lu tion for 10 -60min s under the microwave enviro nment with the microwave pow er being of 500-800 W further comprises comprising: reacting the mixed solution for 5-30mins under the microwave enviro mn ent with the microwa ve power being f 500-800W, then remov ing and Page 3 of 9 A pplic ation Serial Na.:.1/109, 8!7 Fir st Nam ed in ventor: Mingdong ZH ANG SVG 15109817.03-23-2017.J₀SFMV₂EPXXIFW2.CLM.3.svg 0.52 6.32 Black and white the microwave power being of 500--SOfAW: wherei n the a volume of the an add iti onal first solvent is 10%--15 % of a n 4re initi al vo lu e of the first solvent.
11
Dependent← claim 1Lewis acid
(O rig in al) The method of claim 1, wherein the Lewis acid comprises at least one agent selected fr om the group c o nsisti ng of fe rrie chloride, aluminru chloride, zinc chloride, boron trif lu oride, magnesi um chloride, copper chloride and lit hium chl o ride.
12
Dependent← claim 1organic acid
12. (Original) Th e method of claim 1, wherein the organi c acid comprises at least o ne agent selected f rom the group consisting of citric acid gl u conic acid formic acid, ascorbic acid and oxali e acid.
13
Dependent← claim 1Lewis acid
The method of claim 1, w herein in the. sccond dispersion liquid, the a concentration of the m ixt ur e consisting of the solid crude product, the Lewis acid and one of the reducing polyhydroxy aldehyde and the organic acid is 0. f- 1 g/ml.
5
Independentgraphene oxide
The method of c laim 1, wherein the a concentration of y raphemz graphene oxide in the first dispersion liqu id is 2~ 10 mg/nil.
7
Independentgraphene oxidereducing agent
7. (Curren t ly Amended) The m ethod of cla im I wh erein the a weight ratio of the gra ph ene oxide to the reducing ag ent is 1:3- 10.
9
Independentreducing polyhydroxy aldehyde or organic acid
(C u rre n tly Amended) The method of clai m 1, w herein t he a wei g ht ratio of the solid crude product to one of the reducing p olyhydroxy aldeh y de er and organic acid is 1:5 -40,
10
Independentreducing polyhydroxy aldehyde or organic acid
1 0. The method of clai m 1, wherein the red ucing pol yhydroxy aldehyde is glucose or adipaldehyde.
14
IndependentLewis acid
(C rren tly Amended) The method of clai 1, wherein thc a weight of the Lewis acid is 1%--3 % by weigh t of the mixture.
15
Independentgraphene quantum dots
1 5. (Currently Amen ded) The method of clai m 1, w her ein the step of obtain in g the graphene quantum dots after an isolation and a p ur ification frther comprises comprising: treatin g 4 a resultant obtained by stripping for 2 -- 3ho u rs under ultra s onic condition at 120 300W wit h column chromatog rap hy, and ev a porating u nder vac uum rotary evaporation to gi g e generate the purified graphene quantum dots; Page 4 of 9 App lication Serial No.: 15109,87 First Nam ed in vento r: Mingdong ZHJANG Art Unit: 173 6 Res ponse to OQfic e Action;nailed on 01 17/2017 wherein the a sta ti onar y phase of the chromatograp hy colunm is silica gel or pol yac ryla mide. wherein the first developin g solvent consists of is the a m ixed solution of dich lorideni ethane an d m ethanol w ith Pt e a vo lnn e r a tio being of 1:1 -3, and the second developing so l vent is-c onsists of de io nized water. Page 5 of 9
Materials
Materials described outside the worked examples.
graphene oxide
Precursor/Starting Material
reducing agent
Reducing Agent
Process steps
Additional fabrication and treatment steps described in the patent.
1
Microwave Solvothermal
Step 1
Duration
10, 60 min
Process details
purification:
Reported properties
Performance values and ranges asserted in the specification or claims.
Property
Value
Material
Duration
0.2–1 hours
—
—
Patent
Atlas literature
Patent
US 9,663,370
Large-scale preparation method for graphene quantum dots
Mingdong ZHANG
US
Drawings
Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 3
Figure 3 is the fluorescence spectra of graphen e quantum do ts obtained f rom Embo dim ent 2; Fig u re 4 is the fluorescence spectr a of graphene quant um d ots obta i ned from Embodiment 3;
Figure 5
Figure 5 is the fluorescence spectra of gr aphene quantum dot s obtained fr om Embodiment 4. 5 Em bodi m ents To mak e the inven tion clear a nd easy to un derstand, the detailed description for specific exec u tio n m ode of this invention was accomplished combined with the figure. The concrete detai …
Figure 1
Figure 1, in one e m bodi m ent t he nieth od fo r preparing grap h ene quantum d ots in large-scale inc lu des the steps of S 110 step S 140. Step S i 10: adding g raphene oxide to a first solvent and dispersing u nifor m ly to obtain a first dispersion liquid, followed by adding a reducing agent to …
Claims
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
7 independent · 7 dependent
1
Independentgraphene oxidereducing agentreducing polyhydroxy aldehyde or organic acidLewis acid
(Currently Amended) A m eth o d for preparing graphene qua ntum dots [[in]] on a lar ge-scale, the method comprising: dispersi n g graphene oxide un i for m ly in the a first solvent to o btain a fi r st dispersion liquid, adding a reducing agent in to the fi r st dispersion liquid an d dispersing uniformly to give generate a m ixed solution: treating the mixed solution for 1 0- ~60miins u nder ai mic rowa v e en v ironment w ith ahe. power bking at of 500-8 00W, then cool in g and separating t o obtai n th z: a sol i d ac c crude produ ct; mixing onc c f the a reduci n g polyhydroxy aldehyde or an or g anic acid with the solid crude product, following by addin g the a Lewis acid to obtain a mixture, dispers ing the m ixture in a second solvent unifor m ly to obtain a second dispersion liquid; treating putting wherein the second dispersion liquid into with microwaves microwave treatment f r 0.2 -1 hours with tho a microwave p ow er bing of 500- 800 w, then stripping for ?-3 hours un der an u ltrasonic power of 120- 300w, and p urify ing to obtain thc g raphic graphene quantum dots.
2
Dependent← claim 1
2. (Currently Am ended) The method of claim 1, w herei n before the stcp treating tho mixed solution under microwave environment for 10-60mins with the microwave power being 500-800W, i ncludin g a step of ultrasonic stirring, wherein the step of ultrasonic stirring compriing: stirring the mix o d clution under n ltra s oni z ibr 0. 5 1 hours with the ultrasonic power being 120-300W a step of ultrasonic stirring is performed before the step of treating the mixed solution under the microwave environment for 10-60 mins with the microwave power of 500-800W, wherein the step of ultrasonic stirring comprises: stirring the mixed solution with the ultrasonic power of 120-300W for 0.5-4 hours.
4
Dependent← claim 1solvent
The m eth o d of claim 1, wherein the first solvent and the second solvent both c om prises at least one agent selected from the group consisting of water, di m ethoxyethane, an aqueous sol u tion of poly v inyl alcohol, glycerol a lc ohol, po lyhydrox y aldehyde and N- m ethylpy rrolidone.
6
Dependent← claim 1reducing agent
The method of claim 1, wherein the reducing agent comprises at lea s t one agent selected from the group consisting of citric acid, gluco n ic acid, fo rmic acid, ascorb i c acid. oxalic acid, sodi um citrate, so dium gh conate, sodium fo n nate, sodi mn oxalate and sodiu m ascorbate.
8
Dependent← claim 1
The method of claim 1, wherein the step of treating the mixed so lu tion for 10 -60min s under the microwave enviro nment with the microwave pow er being of 500-800 W further comprises comprising: reacting the mixed solution for 5-30mins under the microwave enviro mn ent with the microwa ve power being f 500-800W, then remov ing and Page 3 of 9 A pplic ation Serial Na.:.1/109, 8!7 Fir st Nam ed in ventor: Mingdong ZH ANG SVG 15109817.03-23-2017.J₀SFMV₂EPXXIFW2.CLM.3.svg 0.52 6.32 Black and white the microwave power being of 500--SOfAW: wherei n the a volume of the an add iti onal first solvent is 10%--15 % of a n 4re initi al vo lu e of the first solvent.
11
Dependent← claim 1Lewis acid
(O rig in al) The method of claim 1, wherein the Lewis acid comprises at least one agent selected fr om the group c o nsisti ng of fe rrie chloride, aluminru chloride, zinc chloride, boron trif lu oride, magnesi um chloride, copper chloride and lit hium chl o ride.
12
Dependent← claim 1organic acid
12. (Original) Th e method of claim 1, wherein the organi c acid comprises at least o ne agent selected f rom the group consisting of citric acid gl u conic acid formic acid, ascorbic acid and oxali e acid.
13
Dependent← claim 1Lewis acid
The method of claim 1, w herein in the. sccond dispersion liquid, the a concentration of the m ixt ur e consisting of the solid crude product, the Lewis acid and one of the reducing polyhydroxy aldehyde and the organic acid is 0. f- 1 g/ml.
5
Independentgraphene oxide
The method of c laim 1, wherein the a concentration of y raphemz graphene oxide in the first dispersion liqu id is 2~ 10 mg/nil.
7
Independentgraphene oxidereducing agent
7. (Curren t ly Amended) The m ethod of cla im I wh erein the a weight ratio of the gra ph ene oxide to the reducing ag ent is 1:3- 10.
9
Independentreducing polyhydroxy aldehyde or organic acid
(C u rre n tly Amended) The method of clai m 1, w herein t he a wei g ht ratio of the solid crude product to one of the reducing p olyhydroxy aldeh y de er and organic acid is 1:5 -40,
10
Independentreducing polyhydroxy aldehyde or organic acid
1 0. The method of clai m 1, wherein the red ucing pol yhydroxy aldehyde is glucose or adipaldehyde.
14
IndependentLewis acid
(C rren tly Amended) The method of clai 1, wherein thc a weight of the Lewis acid is 1%--3 % by weigh t of the mixture.
15
Independentgraphene quantum dots
1 5. (Currently Amen ded) The method of clai m 1, w her ein the step of obtain in g the graphene quantum dots after an isolation and a p ur ification frther comprises comprising: treatin g 4 a resultant obtained by stripping for 2 -- 3ho u rs under ultra s onic condition at 120 300W wit h column chromatog rap hy, and ev a porating u nder vac uum rotary evaporation to gi g e generate the purified graphene quantum dots; Page 4 of 9 App lication Serial No.: 15109,87 First Nam ed in vento r: Mingdong ZHJANG Art Unit: 173 6 Res ponse to OQfic e Action;nailed on 01 17/2017 wherein the a sta ti onar y phase of the chromatograp hy colunm is silica gel or pol yac ryla mide. wherein the first developin g solvent consists of is the a m ixed solution of dich lorideni ethane an d m ethanol w ith Pt e a vo lnn e r a tio being of 1:1 -3, and the second developing so l vent is-c onsists of de io nized water. Page 5 of 9
Materials
Materials described outside the worked examples.
graphene oxide
Precursor/Starting Material
reducing agent
Reducing Agent
Process steps
Additional fabrication and treatment steps described in the patent.
1
Microwave Solvothermal
Step 1
Duration
10, 60 min
Process details
purification:
Reported properties
Performance values and ranges asserted in the specification or claims.
Property
Value
Material
Duration
0.2–1 hours
—
—
Patent
Atlas literature
Patent
US 9,663,370
Large-scale preparation method for graphene quantum dots
Mingdong ZHANG
US
Drawings
Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 3
Figure 3 is the fluorescence spectra of graphen e quantum do ts obtained f rom Embo dim ent 2; Fig u re 4 is the fluorescence spectr a of graphene quant um d ots obta i ned from Embodiment 3;
Figure 5
Figure 5 is the fluorescence spectra of gr aphene quantum dot s obtained fr om Embodiment 4. 5 Em bodi m ents To mak e the inven tion clear a nd easy to un derstand, the detailed description for specific exec u tio n m ode of this invention was accomplished combined with the figure. The concrete detai …
Figure 1
Figure 1, in one e m bodi m ent t he nieth od fo r preparing grap h ene quantum d ots in large-scale inc lu des the steps of S 110 step S 140. Step S i 10: adding g raphene oxide to a first solvent and dispersing u nifor m ly to obtain a first dispersion liquid, followed by adding a reducing agent to …
Claims
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
7 independent · 7 dependent
1
Independentgraphene oxidereducing agentreducing polyhydroxy aldehyde or organic acidLewis acid
(Currently Amended) A m eth o d for preparing graphene qua ntum dots [[in]] on a lar ge-scale, the method comprising: dispersi n g graphene oxide un i for m ly in the a first solvent to o btain a fi r st dispersion liquid, adding a reducing agent in to the fi r st dispersion liquid an d dispersing uniformly to give generate a m ixed solution: treating the mixed solution for 1 0- ~60miins u nder ai mic rowa v e en v ironment w ith ahe. power bking at of 500-8 00W, then cool in g and separating t o obtai n th z: a sol i d ac c crude produ ct; mixing onc c f the a reduci n g polyhydroxy aldehyde or an or g anic acid with the solid crude product, following by addin g the a Lewis acid to obtain a mixture, dispers ing the m ixture in a second solvent unifor m ly to obtain a second dispersion liquid; treating putting wherein the second dispersion liquid into with microwaves microwave treatment f r 0.2 -1 hours with tho a microwave p ow er bing of 500- 800 w, then stripping for ?-3 hours un der an u ltrasonic power of 120- 300w, and p urify ing to obtain thc g raphic graphene quantum dots.
2
Dependent← claim 1
2. (Currently Am ended) The method of claim 1, w herei n before the stcp treating tho mixed solution under microwave environment for 10-60mins with the microwave power being 500-800W, i ncludin g a step of ultrasonic stirring, wherein the step of ultrasonic stirring compriing: stirring the mix o d clution under n ltra s oni z ibr 0. 5 1 hours with the ultrasonic power being 120-300W a step of ultrasonic stirring is performed before the step of treating the mixed solution under the microwave environment for 10-60 mins with the microwave power of 500-800W, wherein the step of ultrasonic stirring comprises: stirring the mixed solution with the ultrasonic power of 120-300W for 0.5-4 hours.
4
Dependent← claim 1solvent
The m eth o d of claim 1, wherein the first solvent and the second solvent both c om prises at least one agent selected from the group consisting of water, di m ethoxyethane, an aqueous sol u tion of poly v inyl alcohol, glycerol a lc ohol, po lyhydrox y aldehyde and N- m ethylpy rrolidone.
6
Dependent← claim 1reducing agent
The method of claim 1, wherein the reducing agent comprises at lea s t one agent selected from the group consisting of citric acid, gluco n ic acid, fo rmic acid, ascorb i c acid. oxalic acid, sodi um citrate, so dium gh conate, sodium fo n nate, sodi mn oxalate and sodiu m ascorbate.
8
Dependent← claim 1
The method of claim 1, wherein the step of treating the mixed so lu tion for 10 -60min s under the microwave enviro nment with the microwave pow er being of 500-800 W further comprises comprising: reacting the mixed solution for 5-30mins under the microwave enviro mn ent with the microwa ve power being f 500-800W, then remov ing and Page 3 of 9 A pplic ation Serial Na.:.1/109, 8!7 Fir st Nam ed in ventor: Mingdong ZH ANG SVG 15109817.03-23-2017.J₀SFMV₂EPXXIFW2.CLM.3.svg 0.52 6.32 Black and white the microwave power being of 500--SOfAW: wherei n the a volume of the an add iti onal first solvent is 10%--15 % of a n 4re initi al vo lu e of the first solvent.
11
Dependent← claim 1Lewis acid
(O rig in al) The method of claim 1, wherein the Lewis acid comprises at least one agent selected fr om the group c o nsisti ng of fe rrie chloride, aluminru chloride, zinc chloride, boron trif lu oride, magnesi um chloride, copper chloride and lit hium chl o ride.
12
Dependent← claim 1organic acid
12. (Original) Th e method of claim 1, wherein the organi c acid comprises at least o ne agent selected f rom the group consisting of citric acid gl u conic acid formic acid, ascorbic acid and oxali e acid.
13
Dependent← claim 1Lewis acid
The method of claim 1, w herein in the. sccond dispersion liquid, the a concentration of the m ixt ur e consisting of the solid crude product, the Lewis acid and one of the reducing polyhydroxy aldehyde and the organic acid is 0. f- 1 g/ml.
5
Independentgraphene oxide
The method of c laim 1, wherein the a concentration of y raphemz graphene oxide in the first dispersion liqu id is 2~ 10 mg/nil.
7
Independentgraphene oxidereducing agent
7. (Curren t ly Amended) The m ethod of cla im I wh erein the a weight ratio of the gra ph ene oxide to the reducing ag ent is 1:3- 10.
9
Independentreducing polyhydroxy aldehyde or organic acid
(C u rre n tly Amended) The method of clai m 1, w herein t he a wei g ht ratio of the solid crude product to one of the reducing p olyhydroxy aldeh y de er and organic acid is 1:5 -40,
10
Independentreducing polyhydroxy aldehyde or organic acid
1 0. The method of clai m 1, wherein the red ucing pol yhydroxy aldehyde is glucose or adipaldehyde.
14
IndependentLewis acid
(C rren tly Amended) The method of clai 1, wherein thc a weight of the Lewis acid is 1%--3 % by weigh t of the mixture.
15
Independentgraphene quantum dots
1 5. (Currently Amen ded) The method of clai m 1, w her ein the step of obtain in g the graphene quantum dots after an isolation and a p ur ification frther comprises comprising: treatin g 4 a resultant obtained by stripping for 2 -- 3ho u rs under ultra s onic condition at 120 300W wit h column chromatog rap hy, and ev a porating u nder vac uum rotary evaporation to gi g e generate the purified graphene quantum dots; Page 4 of 9 App lication Serial No.: 15109,87 First Nam ed in vento r: Mingdong ZHJANG Art Unit: 173 6 Res ponse to OQfic e Action;nailed on 01 17/2017 wherein the a sta ti onar y phase of the chromatograp hy colunm is silica gel or pol yac ryla mide. wherein the first developin g solvent consists of is the a m ixed solution of dich lorideni ethane an d m ethanol w ith Pt e a vo lnn e r a tio being of 1:1 -3, and the second developing so l vent is-c onsists of de io nized water. Page 5 of 9
Materials
Materials described outside the worked examples.
graphene oxide
Precursor/Starting Material
reducing agent
Reducing Agent
Process steps
Additional fabrication and treatment steps described in the patent.
1
Microwave Solvothermal
Step 1
Duration
10, 60 min
Process details
purification:
Reported properties
Performance values and ranges asserted in the specification or claims.
column chromatography (silica gel or polyacrylamide); first eluent: dichloromethane/methanol 1:1-3 v/v; second eluent: deionized water; vacuum rotary evaporation
step1 description:Disperse graphene oxide in first solvent; add reducing agent; treat under microwave 500-800W for 10-60 min; cool and separate solid crude product
step2 description:Mix solid crude product with reducing polyhydroxy aldehyde or organic acid and Lewis acid in second solvent; microwave treatment 500-800W for 0.2-1 h; ultrasonic stripping 120-300W for 2-3 h; purify
temperature c max:800
temperature c min:500
step2 microwave time h:0.2-1
step1 microwave power W:500-800
step2 microwave power W:500-800
step2 ultrasonic time h:2-3
step1 microwave time min:10-60
step2 ultrasonic power W:120-300
lewis acid wt percent of mixture:1-3
graphene oxide concentration mg per mL:2-10
graphene oxide to reducing agent weight ratio:1:3-10
mixture concentration in second dispersion g per mL:0.1-1
solid crude to polyhydroxy aldehyde or organic acid weight ratio:1:5-40
column chromatography (silica gel or polyacrylamide); first eluent: dichloromethane/methanol 1:1-3 v/v; second eluent: deionized water; vacuum rotary evaporation
step1 description:Disperse graphene oxide in first solvent; add reducing agent; treat under microwave 500-800W for 10-60 min; cool and separate solid crude product
step2 description:Mix solid crude product with reducing polyhydroxy aldehyde or organic acid and Lewis acid in second solvent; microwave treatment 500-800W for 0.2-1 h; ultrasonic stripping 120-300W for 2-3 h; purify
temperature c max:800
temperature c min:500
step2 microwave time h:0.2-1
step1 microwave power W:500-800
step2 microwave power W:500-800
step2 ultrasonic time h:2-3
step1 microwave time min:10-60
step2 ultrasonic power W:120-300
lewis acid wt percent of mixture:1-3
graphene oxide concentration mg per mL:2-10
graphene oxide to reducing agent weight ratio:1:3-10
mixture concentration in second dispersion g per mL:0.1-1
solid crude to polyhydroxy aldehyde or organic acid weight ratio:1:5-40
column chromatography (silica gel or polyacrylamide); first eluent: dichloromethane/methanol 1:1-3 v/v; second eluent: deionized water; vacuum rotary evaporation
step1 description:Disperse graphene oxide in first solvent; add reducing agent; treat under microwave 500-800W for 10-60 min; cool and separate solid crude product
step2 description:Mix solid crude product with reducing polyhydroxy aldehyde or organic acid and Lewis acid in second solvent; microwave treatment 500-800W for 0.2-1 h; ultrasonic stripping 120-300W for 2-3 h; purify
temperature c max:800
temperature c min:500
step2 microwave time h:0.2-1
step1 microwave power W:500-800
step2 microwave power W:500-800
step2 ultrasonic time h:2-3
step1 microwave time min:10-60
step2 ultrasonic power W:120-300
lewis acid wt percent of mixture:1-3
graphene oxide concentration mg per mL:2-10
graphene oxide to reducing agent weight ratio:1:3-10
mixture concentration in second dispersion g per mL:0.1-1
solid crude to polyhydroxy aldehyde or organic acid weight ratio:1:5-40
column chromatography (silica gel or polyacrylamide); first eluent: dichloromethane/methanol 1:1-3 v/v; second eluent: deionized water; vacuum rotary evaporation
step1 description:Disperse graphene oxide in first solvent; add reducing agent; treat under microwave 500-800W for 10-60 min; cool and separate solid crude product
step2 description:Mix solid crude product with reducing polyhydroxy aldehyde or organic acid and Lewis acid in second solvent; microwave treatment 500-800W for 0.2-1 h; ultrasonic stripping 120-300W for 2-3 h; purify
temperature c max:800
temperature c min:500
step2 microwave time h:0.2-1
step1 microwave power W:500-800
step2 microwave power W:500-800
step2 ultrasonic time h:2-3
step1 microwave time min:10-60
step2 ultrasonic power W:120-300
lewis acid wt percent of mixture:1-3
graphene oxide concentration mg per mL:2-10
graphene oxide to reducing agent weight ratio:1:3-10
mixture concentration in second dispersion g per mL:0.1-1
solid crude to polyhydroxy aldehyde or organic acid weight ratio:1:5-40