Patent
US 10,030,155NOVEL GRAPHENE NANODISPERSION AND METHOD FOR PREPARING SAME
Takuzo Aida
US
Copyright © 2026 Matter42. All rights reserved.
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US 10,030,155Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1] Raman spectrum of graphene powder obtained from a graphene dispersion using graphite powder and the ionic liquid (compound 1) of the present invention. …
FIG. 2] Distribution of number of graphene layers in graphite. [
FIG. 3] Distribution of number of graphene layers in a graphene dispersion obtained by microwave treatment using compound 1. [
FIG. 4] Distribution of number of graphene layers in a graphene dispersion obtained by ultrasonication using compound 1. 7 [
FIG. 5] Distribution of number of graphene layers in a graphene dispersion obtained by microwave treatment using compound 3. [
FIG. 6] Distribution of number of graphene layers in a graphene dispersion obtained by microwave treatment using BMI PF6. [
FIG. 7] Dynamic viscoelastic properties of a dispersion before and after microwave treatment using compound 1. BEST MODE FOR CARRYING OUT THE INVENTION [0015] …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
An ionic liquid represented by the following general formula (1): SVG 14400877.02-08-2018.JDEWZD₂KRXEAPX0.CLM.1.7.782.807.1661.1088.svg 0.937 2.93 Chemistry Black and white (1) wherein R 1 and R 5 may be the same or different and each independently represent a substituted or unsubstituted C 1 _ 7 linear or branched alkyl group, R 2 is represented by the following formula (2): R 6 -O SVG 14400877.02-08-2018.JDEWZD₂KRXEAPX0.CLM.1.12.1234.1590.1332.1716.svg 0.42 0.327 Chemistry Black and white R 7 SVG 14400877.02-08-2018.JDEWZD₂KRXEAPX0.CLM.1.12.917.1589.1017.1710.svg 0.403 0.333 Chemistry Black and white SVG 14400877.02-08-2018.JDEWZD₂KRXEAPX0.CLM.1.13.1578.1705.1637.1736.svg 0.103 0.197 Chemistry Black and white wherein R 6 and R 7 may be the same or different and each independently represent a C 1 _ 4 linear or branched alkylene group, m represents an integer of 2 or 3, R 3 and R 4 may be the same or different and each independently represent a hydrogen atom, substituted or unsubstituted C 1 _ 4 linear or branched alkyl group, X- represents a counter ion, n represents 1-30. Previously presented
The ionic liquid according to Claim 1, wherein R 1 and R 5 are C 1 _ 6 linear alkyls. Previously presented
The ionic liquid according to Claim 1, wherein R 6 and R 7 are both ethylene groups. Previously presented
The ionic liquid according to Claim 1, wherein n is an integer of 1-2. Previously presented
The ionic liquid according to Claim 1, wherein X-is selected from the g rou p consistin g of PF & (CF 3 SO 2) 2 N -4, B F 4-, C l-, and Br. SVG 14400877.02-08-2018.JDEWZD₂KRXEAPX0.CLM.2.4.1110.479.1147.503.svg 0.08 0.123 Chemistry Black and white Currently amended
An ionic liquid mixture comprising the ionic liquid (A) according to Claim 1 and butylmethylimidazolium hexafluorophosphate (B) or butylmethylimidazolium bis(trifluoromethanesulfonyl)imide (C). Withdrawn
A graphene dispersion comprising graphene and the ionic liquid according to Claim 1 or an ionic liquid mixture comprising the ionic liquid (A) according to Claim 1 and butylmethylimidazolium hexafluorophosphate (B) or butylmethylimidazolium bis(trifluoromethanesulfonyl)imide (C). Withdrawn
A method for preparing a graphene dispersion comprising: (1) adding graphite to the ionic liquid according to Claim 1 or an ionic liquid mixture comprising the ionic liquid (A) according to Claim 1 and butylmethylimidazolium hexafluorophosphate (B) or butylmethylimidazolium bis(trifluoromethanesulfonyl)imide (C), and (2) applying ultrasound or microwaves to the mixture obtained in (1). Withdrawn
Embodiments described in the patent, grouped by the materials and process steps they use.
3 materials1 process step
Synthesis of compound 1a: 1-Butylimidazole (37.15 g, 0.299 mol) was added to an acetonitrile solution (40 mL) of triethylene glycol bis(p-toluenesulfonic acid ester) (62.36 g, 0.136 mol) under an argon atmosphere and mixed for 72 hours at 60°C. After concentration under reduced pressure and drying, methylene chloride (10 mL) was added and two-layer separation was carried out three times with ethyl acetate (50 mL). Compound 1a (57 g, 0.129 mol, yield: 81%), a pale yellow viscous liquid, was obtained by drying the ionic liquid layer by rotary evaporator and vacuum oven overnight at 105°C with P₂O5.
2 materials1 process step
Synthesis of compound 1: Aqueous solution of KPF₆ (23 g, 0.125 mol) was added to an acetonitrile solution (30 mL) of compound 1a (38.17 g, 0.054 mol) and stirred for two hours at room temperature. After phase separation, the ionic liquid layer was washed three times with distilled water (30 mL), dried over Na₂SO4, concentrated by rotary evaporator, and dried overnight in vacuum oven at 105°C with P₂O5. Compound 1 (30.3 g, 0.046 mol, yield: 85%), a viscous liquid, was obtained.
Materials described outside the worked examples.
bis-imidazolium ionic liquid (general formula 1)
butylmethylimidazolium hexafluorophosphate
butylmethylimidazolium bis(trifluoromethanesulfonyl)imide
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 1] Raman spectrum of graphene powder obtained from a graphene dispersion using graphite powder and the ionic liquid (compound 1) of the present invention. …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Thickness | 2600–2800 cm | — |
Table 1
Table 1 I onic liquid
Table 1 shows the results of measurement of the graphene concentrat
p. 11
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Patent
Atlas literature
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US 10,030,155Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1] Raman spectrum of graphene powder obtained from a graphene dispersion using graphite powder and the ionic liquid (compound 1) of the present invention. …
FIG. 2] Distribution of number of graphene layers in graphite. [
FIG. 3] Distribution of number of graphene layers in a graphene dispersion obtained by microwave treatment using compound 1. [
FIG. 4] Distribution of number of graphene layers in a graphene dispersion obtained by ultrasonication using compound 1. 7 [
FIG. 5] Distribution of number of graphene layers in a graphene dispersion obtained by microwave treatment using compound 3. [
FIG. 6] Distribution of number of graphene layers in a graphene dispersion obtained by microwave treatment using BMI PF6. [
FIG. 7] Dynamic viscoelastic properties of a dispersion before and after microwave treatment using compound 1. BEST MODE FOR CARRYING OUT THE INVENTION [0015] …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
An ionic liquid represented by the following general formula (1): SVG 14400877.02-08-2018.JDEWZD₂KRXEAPX0.CLM.1.7.782.807.1661.1088.svg 0.937 2.93 Chemistry Black and white (1) wherein R 1 and R 5 may be the same or different and each independently represent a substituted or unsubstituted C 1 _ 7 linear or branched alkyl group, R 2 is represented by the following formula (2): R 6 -O SVG 14400877.02-08-2018.JDEWZD₂KRXEAPX0.CLM.1.12.1234.1590.1332.1716.svg 0.42 0.327 Chemistry Black and white R 7 SVG 14400877.02-08-2018.JDEWZD₂KRXEAPX0.CLM.1.12.917.1589.1017.1710.svg 0.403 0.333 Chemistry Black and white SVG 14400877.02-08-2018.JDEWZD₂KRXEAPX0.CLM.1.13.1578.1705.1637.1736.svg 0.103 0.197 Chemistry Black and white wherein R 6 and R 7 may be the same or different and each independently represent a C 1 _ 4 linear or branched alkylene group, m represents an integer of 2 or 3, R 3 and R 4 may be the same or different and each independently represent a hydrogen atom, substituted or unsubstituted C 1 _ 4 linear or branched alkyl group, X- represents a counter ion, n represents 1-30. Previously presented
The ionic liquid according to Claim 1, wherein R 1 and R 5 are C 1 _ 6 linear alkyls. Previously presented
The ionic liquid according to Claim 1, wherein R 6 and R 7 are both ethylene groups. Previously presented
The ionic liquid according to Claim 1, wherein n is an integer of 1-2. Previously presented
The ionic liquid according to Claim 1, wherein X-is selected from the g rou p consistin g of PF & (CF 3 SO 2) 2 N -4, B F 4-, C l-, and Br. SVG 14400877.02-08-2018.JDEWZD₂KRXEAPX0.CLM.2.4.1110.479.1147.503.svg 0.08 0.123 Chemistry Black and white Currently amended
An ionic liquid mixture comprising the ionic liquid (A) according to Claim 1 and butylmethylimidazolium hexafluorophosphate (B) or butylmethylimidazolium bis(trifluoromethanesulfonyl)imide (C). Withdrawn
A graphene dispersion comprising graphene and the ionic liquid according to Claim 1 or an ionic liquid mixture comprising the ionic liquid (A) according to Claim 1 and butylmethylimidazolium hexafluorophosphate (B) or butylmethylimidazolium bis(trifluoromethanesulfonyl)imide (C). Withdrawn
A method for preparing a graphene dispersion comprising: (1) adding graphite to the ionic liquid according to Claim 1 or an ionic liquid mixture comprising the ionic liquid (A) according to Claim 1 and butylmethylimidazolium hexafluorophosphate (B) or butylmethylimidazolium bis(trifluoromethanesulfonyl)imide (C), and (2) applying ultrasound or microwaves to the mixture obtained in (1). Withdrawn
Embodiments described in the patent, grouped by the materials and process steps they use.
3 materials1 process step
Synthesis of compound 1a: 1-Butylimidazole (37.15 g, 0.299 mol) was added to an acetonitrile solution (40 mL) of triethylene glycol bis(p-toluenesulfonic acid ester) (62.36 g, 0.136 mol) under an argon atmosphere and mixed for 72 hours at 60°C. After concentration under reduced pressure and drying, methylene chloride (10 mL) was added and two-layer separation was carried out three times with ethyl acetate (50 mL). Compound 1a (57 g, 0.129 mol, yield: 81%), a pale yellow viscous liquid, was obtained by drying the ionic liquid layer by rotary evaporator and vacuum oven overnight at 105°C with P₂O5.
2 materials1 process step
Synthesis of compound 1: Aqueous solution of KPF₆ (23 g, 0.125 mol) was added to an acetonitrile solution (30 mL) of compound 1a (38.17 g, 0.054 mol) and stirred for two hours at room temperature. After phase separation, the ionic liquid layer was washed three times with distilled water (30 mL), dried over Na₂SO4, concentrated by rotary evaporator, and dried overnight in vacuum oven at 105°C with P₂O5. Compound 1 (30.3 g, 0.046 mol, yield: 85%), a viscous liquid, was obtained.
Materials described outside the worked examples.
bis-imidazolium ionic liquid (general formula 1)
butylmethylimidazolium hexafluorophosphate
butylmethylimidazolium bis(trifluoromethanesulfonyl)imide
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 1] Raman spectrum of graphene powder obtained from a graphene dispersion using graphite powder and the ionic liquid (compound 1) of the present invention. …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Thickness | 2600–2800 cm | — |
Table 1
Table 1 I onic liquid
Table 1 shows the results of measurement of the graphene concentrat
p. 11
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 10,030,155Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1] Raman spectrum of graphene powder obtained from a graphene dispersion using graphite powder and the ionic liquid (compound 1) of the present invention. …
FIG. 2] Distribution of number of graphene layers in graphite. [
FIG. 3] Distribution of number of graphene layers in a graphene dispersion obtained by microwave treatment using compound 1. [
FIG. 4] Distribution of number of graphene layers in a graphene dispersion obtained by ultrasonication using compound 1. 7 [
FIG. 5] Distribution of number of graphene layers in a graphene dispersion obtained by microwave treatment using compound 3. [
FIG. 6] Distribution of number of graphene layers in a graphene dispersion obtained by microwave treatment using BMI PF6. [
FIG. 7] Dynamic viscoelastic properties of a dispersion before and after microwave treatment using compound 1. BEST MODE FOR CARRYING OUT THE INVENTION [0015] …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
An ionic liquid represented by the following general formula (1): SVG 14400877.02-08-2018.JDEWZD₂KRXEAPX0.CLM.1.7.782.807.1661.1088.svg 0.937 2.93 Chemistry Black and white (1) wherein R 1 and R 5 may be the same or different and each independently represent a substituted or unsubstituted C 1 _ 7 linear or branched alkyl group, R 2 is represented by the following formula (2): R 6 -O SVG 14400877.02-08-2018.JDEWZD₂KRXEAPX0.CLM.1.12.1234.1590.1332.1716.svg 0.42 0.327 Chemistry Black and white R 7 SVG 14400877.02-08-2018.JDEWZD₂KRXEAPX0.CLM.1.12.917.1589.1017.1710.svg 0.403 0.333 Chemistry Black and white SVG 14400877.02-08-2018.JDEWZD₂KRXEAPX0.CLM.1.13.1578.1705.1637.1736.svg 0.103 0.197 Chemistry Black and white wherein R 6 and R 7 may be the same or different and each independently represent a C 1 _ 4 linear or branched alkylene group, m represents an integer of 2 or 3, R 3 and R 4 may be the same or different and each independently represent a hydrogen atom, substituted or unsubstituted C 1 _ 4 linear or branched alkyl group, X- represents a counter ion, n represents 1-30. Previously presented
The ionic liquid according to Claim 1, wherein R 1 and R 5 are C 1 _ 6 linear alkyls. Previously presented
The ionic liquid according to Claim 1, wherein R 6 and R 7 are both ethylene groups. Previously presented
The ionic liquid according to Claim 1, wherein n is an integer of 1-2. Previously presented
The ionic liquid according to Claim 1, wherein X-is selected from the g rou p consistin g of PF & (CF 3 SO 2) 2 N -4, B F 4-, C l-, and Br. SVG 14400877.02-08-2018.JDEWZD₂KRXEAPX0.CLM.2.4.1110.479.1147.503.svg 0.08 0.123 Chemistry Black and white Currently amended
An ionic liquid mixture comprising the ionic liquid (A) according to Claim 1 and butylmethylimidazolium hexafluorophosphate (B) or butylmethylimidazolium bis(trifluoromethanesulfonyl)imide (C). Withdrawn
A graphene dispersion comprising graphene and the ionic liquid according to Claim 1 or an ionic liquid mixture comprising the ionic liquid (A) according to Claim 1 and butylmethylimidazolium hexafluorophosphate (B) or butylmethylimidazolium bis(trifluoromethanesulfonyl)imide (C). Withdrawn
A method for preparing a graphene dispersion comprising: (1) adding graphite to the ionic liquid according to Claim 1 or an ionic liquid mixture comprising the ionic liquid (A) according to Claim 1 and butylmethylimidazolium hexafluorophosphate (B) or butylmethylimidazolium bis(trifluoromethanesulfonyl)imide (C), and (2) applying ultrasound or microwaves to the mixture obtained in (1). Withdrawn
Embodiments described in the patent, grouped by the materials and process steps they use.
3 materials1 process step
Synthesis of compound 1a: 1-Butylimidazole (37.15 g, 0.299 mol) was added to an acetonitrile solution (40 mL) of triethylene glycol bis(p-toluenesulfonic acid ester) (62.36 g, 0.136 mol) under an argon atmosphere and mixed for 72 hours at 60°C. After concentration under reduced pressure and drying, methylene chloride (10 mL) was added and two-layer separation was carried out three times with ethyl acetate (50 mL). Compound 1a (57 g, 0.129 mol, yield: 81%), a pale yellow viscous liquid, was obtained by drying the ionic liquid layer by rotary evaporator and vacuum oven overnight at 105°C with P₂O5.
2 materials1 process step
Synthesis of compound 1: Aqueous solution of KPF₆ (23 g, 0.125 mol) was added to an acetonitrile solution (30 mL) of compound 1a (38.17 g, 0.054 mol) and stirred for two hours at room temperature. After phase separation, the ionic liquid layer was washed three times with distilled water (30 mL), dried over Na₂SO4, concentrated by rotary evaporator, and dried overnight in vacuum oven at 105°C with P₂O5. Compound 1 (30.3 g, 0.046 mol, yield: 85%), a viscous liquid, was obtained.
Materials described outside the worked examples.
bis-imidazolium ionic liquid (general formula 1)
butylmethylimidazolium hexafluorophosphate
butylmethylimidazolium bis(trifluoromethanesulfonyl)imide
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 1] Raman spectrum of graphene powder obtained from a graphene dispersion using graphite powder and the ionic liquid (compound 1) of the present invention. …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Thickness | 2600–2800 cm | — |
Table 1
Table 1 I onic liquid
Table 1 shows the results of measurement of the graphene concentrat
p. 11
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 10,030,155Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1] Raman spectrum of graphene powder obtained from a graphene dispersion using graphite powder and the ionic liquid (compound 1) of the present invention. …
FIG. 2] Distribution of number of graphene layers in graphite. [
FIG. 3] Distribution of number of graphene layers in a graphene dispersion obtained by microwave treatment using compound 1. [
FIG. 4] Distribution of number of graphene layers in a graphene dispersion obtained by ultrasonication using compound 1. 7 [
FIG. 5] Distribution of number of graphene layers in a graphene dispersion obtained by microwave treatment using compound 3. [
FIG. 6] Distribution of number of graphene layers in a graphene dispersion obtained by microwave treatment using BMI PF6. [
FIG. 7] Dynamic viscoelastic properties of a dispersion before and after microwave treatment using compound 1. BEST MODE FOR CARRYING OUT THE INVENTION [0015] …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
An ionic liquid represented by the following general formula (1): SVG 14400877.02-08-2018.JDEWZD₂KRXEAPX0.CLM.1.7.782.807.1661.1088.svg 0.937 2.93 Chemistry Black and white (1) wherein R 1 and R 5 may be the same or different and each independently represent a substituted or unsubstituted C 1 _ 7 linear or branched alkyl group, R 2 is represented by the following formula (2): R 6 -O SVG 14400877.02-08-2018.JDEWZD₂KRXEAPX0.CLM.1.12.1234.1590.1332.1716.svg 0.42 0.327 Chemistry Black and white R 7 SVG 14400877.02-08-2018.JDEWZD₂KRXEAPX0.CLM.1.12.917.1589.1017.1710.svg 0.403 0.333 Chemistry Black and white SVG 14400877.02-08-2018.JDEWZD₂KRXEAPX0.CLM.1.13.1578.1705.1637.1736.svg 0.103 0.197 Chemistry Black and white wherein R 6 and R 7 may be the same or different and each independently represent a C 1 _ 4 linear or branched alkylene group, m represents an integer of 2 or 3, R 3 and R 4 may be the same or different and each independently represent a hydrogen atom, substituted or unsubstituted C 1 _ 4 linear or branched alkyl group, X- represents a counter ion, n represents 1-30. Previously presented
The ionic liquid according to Claim 1, wherein R 1 and R 5 are C 1 _ 6 linear alkyls. Previously presented
The ionic liquid according to Claim 1, wherein R 6 and R 7 are both ethylene groups. Previously presented
The ionic liquid according to Claim 1, wherein n is an integer of 1-2. Previously presented
The ionic liquid according to Claim 1, wherein X-is selected from the g rou p consistin g of PF & (CF 3 SO 2) 2 N -4, B F 4-, C l-, and Br. SVG 14400877.02-08-2018.JDEWZD₂KRXEAPX0.CLM.2.4.1110.479.1147.503.svg 0.08 0.123 Chemistry Black and white Currently amended
An ionic liquid mixture comprising the ionic liquid (A) according to Claim 1 and butylmethylimidazolium hexafluorophosphate (B) or butylmethylimidazolium bis(trifluoromethanesulfonyl)imide (C). Withdrawn
A graphene dispersion comprising graphene and the ionic liquid according to Claim 1 or an ionic liquid mixture comprising the ionic liquid (A) according to Claim 1 and butylmethylimidazolium hexafluorophosphate (B) or butylmethylimidazolium bis(trifluoromethanesulfonyl)imide (C). Withdrawn
A method for preparing a graphene dispersion comprising: (1) adding graphite to the ionic liquid according to Claim 1 or an ionic liquid mixture comprising the ionic liquid (A) according to Claim 1 and butylmethylimidazolium hexafluorophosphate (B) or butylmethylimidazolium bis(trifluoromethanesulfonyl)imide (C), and (2) applying ultrasound or microwaves to the mixture obtained in (1). Withdrawn
Embodiments described in the patent, grouped by the materials and process steps they use.
3 materials1 process step
Synthesis of compound 1a: 1-Butylimidazole (37.15 g, 0.299 mol) was added to an acetonitrile solution (40 mL) of triethylene glycol bis(p-toluenesulfonic acid ester) (62.36 g, 0.136 mol) under an argon atmosphere and mixed for 72 hours at 60°C. After concentration under reduced pressure and drying, methylene chloride (10 mL) was added and two-layer separation was carried out three times with ethyl acetate (50 mL). Compound 1a (57 g, 0.129 mol, yield: 81%), a pale yellow viscous liquid, was obtained by drying the ionic liquid layer by rotary evaporator and vacuum oven overnight at 105°C with P₂O5.
2 materials1 process step
Synthesis of compound 1: Aqueous solution of KPF₆ (23 g, 0.125 mol) was added to an acetonitrile solution (30 mL) of compound 1a (38.17 g, 0.054 mol) and stirred for two hours at room temperature. After phase separation, the ionic liquid layer was washed three times with distilled water (30 mL), dried over Na₂SO4, concentrated by rotary evaporator, and dried overnight in vacuum oven at 105°C with P₂O5. Compound 1 (30.3 g, 0.046 mol, yield: 85%), a viscous liquid, was obtained.
Materials described outside the worked examples.
bis-imidazolium ionic liquid (general formula 1)
butylmethylimidazolium hexafluorophosphate
butylmethylimidazolium bis(trifluoromethanesulfonyl)imide
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 1] Raman spectrum of graphene powder obtained from a graphene dispersion using graphite powder and the ionic liquid (compound 1) of the present invention. …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Thickness | 2600–2800 cm | — |
Table 1
Table 1 I onic liquid
Table 1 shows the results of measurement of the graphene concentrat
p. 11
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