CN108298533A - A method of preparing graphene oxide solution - Google Patents
A method of preparing graphene oxide solution Download PDFInfo
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- CN108298533A CN108298533A CN201810344209.8A CN201810344209A CN108298533A CN 108298533 A CN108298533 A CN 108298533A CN 201810344209 A CN201810344209 A CN 201810344209A CN 108298533 A CN108298533 A CN 108298533A
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- water
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/22—Electronic properties
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Abstract
A method of graphene oxide solution is prepared, including:Step 1:At room temperature, the salpeter solution of the concentrated sulfuric acid of 70mL98wt% and 5ml25wt% are mixed, is then slowly added to 3.0g graphite powders while stirring, is added followed by 1.5g sodium nitrate and 1.1g niter cakes;Step 2:This mixture is moved into cooling in ice bath, under violent stirring, is slowly added into 9.0g potassium permanganate and 1g potassium nitrate.
Description
Technical field
The present invention relates to a kind of methods preparing graphene oxide solution.
Background technology
The method flow in the prior art for preparing graphene oxide solution is complicated, low precision, not environmentally.
Invention content
A method of graphene oxide solution is prepared, including:
Step 1:At room temperature, the salpeter solution of the concentrated sulfuric acid of 70mL98wt% and 5ml25wt% are mixed, is then delayed while stirring
It is slow that 3.0g graphite powders are added, it is added followed by 1.5g sodium nitrate and 1.1g niter cakes;
Step 2:This mixture is moved into cooling in ice bath, under violent stirring, is slowly added into 9.0g potassium permanganate and 1g
Potassium nitrate;
Step 3:After charging, reaction system is transferred in 40 °C of water-baths, constant temperature stirring is reacted 30 minutes;
Step 4:150mL deionized waters are slowly added to, and water-bath is warming up to 90 °C, are reacted 15 minutes;
Step 5:500mL water is added, the hydrogen peroxide of 15mL30wt% is slowly added to;
Step 6:The mixture of gained filter and washed with the dilute hydrochloric acid of 250mL3.5wt% to remove metal ion,
It is washed with 200mL deionized waters again to remove the acid of remaining;
Step 7:It is diluted in input deionized water after solid filter cake is dried in air, graphite oxide is obtained by being ultrasonically treated
Alkene dispersion liquid;
Step 8:This dispersion liquid is fitted into and is dialysed in bag filter to remove the acid and metal ion of remaining, is changed daily primary
Water is dialysed seven days;
Step 9:Graphene oxide dispersion after dialysis is taken out and is centrifuged under the conditions of 4000 rpms, discards lower layer not
The graphite powder of oxidation or non-complete oxidation collects upper solution.
The graphene oxide solution of the present invention can be applied to field of cell preparation.
Inventive point is:1)Complete reaction process;2)Material used;3)Concrete component.
Specific implementation mode
Embodiment 1
A method of graphene oxide solution is prepared, including:
Step 1:At room temperature, the salpeter solution of the concentrated sulfuric acid of 70mL98wt% and 5ml25wt% are mixed, is then delayed while stirring
It is slow that 3.0g graphite powders are added, it is added followed by 1.5g sodium nitrate and 1.1g niter cakes;
Step 2:This mixture is moved into cooling in ice bath, under violent stirring, is slowly added into 9.0g potassium permanganate and 1g
Potassium nitrate;
Step 3:After charging, reaction system is transferred in 40 °C of water-baths, constant temperature stirring is reacted 30 minutes;
Step 4:150mL deionized waters are slowly added to, and water-bath is warming up to 90 °C, are reacted 15 minutes;
Step 5:500mL water is added, the hydrogen peroxide of 15mL30wt% is slowly added to;
Step 6:The mixture of gained filter and washed with the dilute hydrochloric acid of 250mL3.5wt% to remove metal ion,
It is washed with 200mL deionized waters again to remove the acid of remaining;
Step 7:It is diluted in input deionized water after solid filter cake is dried in air, graphite oxide is obtained by being ultrasonically treated
Alkene dispersion liquid;
Step 8:This dispersion liquid is fitted into and is dialysed in bag filter to remove the acid and metal ion of remaining, is changed daily primary
Water is dialysed seven days;
Step 9:Graphene oxide dispersion after dialysis is taken out and is centrifuged under the conditions of 4000 rpms, discards lower layer not
The graphite powder of oxidation or non-complete oxidation collects upper solution.
The graphene oxide solution of the present invention can be applied to field of cell preparation.
Embodiment 2
A method of graphene oxide solution is prepared, including:
Step 1:At room temperature, the salpeter solution of the concentrated sulfuric acid of 70mL98wt% and 5ml25wt% are mixed, is then delayed while stirring
It is slow that 3.0g graphite powders are added, it is added followed by 1.5g sodium nitrate and 1.2g niter cakes;
Step 2:This mixture is moved into cooling in ice bath, under violent stirring, is slowly added into 9.0g potassium permanganate and 1g
Potassium nitrate;
Step 3:After charging, reaction system is transferred in 40 °C of water-baths, constant temperature stirring is reacted 30 minutes;
Step 4:150mL deionized waters are slowly added to, and water-bath is warming up to 90 °C, are reacted 15 minutes;
Step 5:500mL water is added, the hydrogen peroxide of 15mL30wt% is slowly added to;
Step 6:The mixture of gained filter and washed with the dilute hydrochloric acid of 250mL3.5wt% to remove metal ion,
It is washed with 200mL deionized waters again to remove the acid of remaining;
Step 7:It is diluted in input deionized water after solid filter cake is dried in air, graphite oxide is obtained by being ultrasonically treated
Alkene dispersion liquid;
Step 8:This dispersion liquid is fitted into and is dialysed in bag filter to remove the acid and metal ion of remaining, is changed daily primary
Water is dialysed seven days;
Step 9:Graphene oxide dispersion after dialysis is taken out and is centrifuged under the conditions of 4000 rpms, discards lower layer not
The graphite powder of oxidation or non-complete oxidation collects upper solution.
The graphene oxide solution of the present invention can be applied to field of cell preparation.
Embodiment 3
A method of graphene oxide solution is prepared, including:
Step 1:At room temperature, the salpeter solution of the concentrated sulfuric acid of 70mL98wt% and 5ml25wt% are mixed, is then delayed while stirring
It is slow that 3.0g graphite powders are added, it is added followed by 1.5g sodium nitrate and 1.3g niter cakes;
Step 2:This mixture is moved into cooling in ice bath, under violent stirring, is slowly added into 9.0g potassium permanganate and 1g
Potassium nitrate;
Step 3:After charging, reaction system is transferred in 40 °C of water-baths, constant temperature stirring is reacted 30 minutes;
Step 4:150mL deionized waters are slowly added to, and water-bath is warming up to 90 °C, are reacted 15 minutes;
Step 5:500mL water is added, the hydrogen peroxide of 15mL30wt% is slowly added to;
Step 6:The mixture of gained filter and washed with the dilute hydrochloric acid of 250mL3.5wt% to remove metal ion,
It is washed with 200mL deionized waters again to remove the acid of remaining;
Step 7:It is diluted in input deionized water after solid filter cake is dried in air, graphite oxide is obtained by being ultrasonically treated
Alkene dispersion liquid;
Step 8:This dispersion liquid is fitted into and is dialysed in bag filter to remove the acid and metal ion of remaining, is changed daily primary
Water is dialysed seven days;
Step 9:Graphene oxide dispersion after dialysis is taken out and is centrifuged under the conditions of 4000 rpms, discards lower layer not
The graphite powder of oxidation or non-complete oxidation collects upper solution.
The graphene oxide solution of the present invention can be applied to field of cell preparation.
Embodiment 4
A method of graphene oxide solution is prepared, including:
Step 1:At room temperature, the salpeter solution of the concentrated sulfuric acid of 70mL98wt% and 5ml25wt% are mixed, is then delayed while stirring
It is slow that 3.0g graphite powders are added, it is added followed by 1.5g sodium nitrate and 1.4g niter cakes;
Step 2:This mixture is moved into cooling in ice bath, under violent stirring, is slowly added into 9.0g potassium permanganate and 1g
Potassium nitrate;
Step 3:After charging, reaction system is transferred in 40 °C of water-baths, constant temperature stirring is reacted 30 minutes;
Step 4:150mL deionized waters are slowly added to, and water-bath is warming up to 90 °C, are reacted 15 minutes;
Step 5:500mL water is added, the hydrogen peroxide of 15mL30wt% is slowly added to;
Step 6:The mixture of gained filter and washed with the dilute hydrochloric acid of 250mL3.5wt% to remove metal ion,
It is washed with 200mL deionized waters again to remove the acid of remaining;
Step 7:It is diluted in input deionized water after solid filter cake is dried in air, graphite oxide is obtained by being ultrasonically treated
Alkene dispersion liquid;
Step 8:This dispersion liquid is fitted into and is dialysed in bag filter to remove the acid and metal ion of remaining, is changed daily primary
Water is dialysed seven days;
Step 9:Graphene oxide dispersion after dialysis is taken out and is centrifuged under the conditions of 4000 rpms, discards lower layer not
The graphite powder of oxidation or non-complete oxidation collects upper solution.
The graphene oxide solution of the present invention can be applied to field of cell preparation.
Embodiment 5
A method of graphene oxide solution is prepared, including:
Step 1:At room temperature, the salpeter solution of the concentrated sulfuric acid of 70mL98wt% and 5ml25wt% are mixed, is then delayed while stirring
It is slow that 3.0g graphite powders are added, it is added followed by 1.5g sodium nitrate and 1.5g niter cakes;
Step 2:This mixture is moved into cooling in ice bath, under violent stirring, is slowly added into 9.0g potassium permanganate and 1g
Potassium nitrate;
Step 3:After charging, reaction system is transferred in 40 °C of water-baths, constant temperature stirring is reacted 30 minutes;
Step 4:150mL deionized waters are slowly added to, and water-bath is warming up to 90 °C, are reacted 15 minutes;
Step 5:500mL water is added, the hydrogen peroxide of 15mL30wt% is slowly added to;
Step 6:The mixture of gained filter and washed with the dilute hydrochloric acid of 250mL3.5wt% to remove metal ion,
It is washed with 200mL deionized waters again to remove the acid of remaining;
Step 7:It is diluted in input deionized water after solid filter cake is dried in air, graphite oxide is obtained by being ultrasonically treated
Alkene dispersion liquid;
Step 8:This dispersion liquid is fitted into and is dialysed in bag filter to remove the acid and metal ion of remaining, is changed daily primary
Water is dialysed seven days;
Step 9:Graphene oxide dispersion after dialysis is taken out and is centrifuged under the conditions of 4000 rpms, discards lower layer not
The graphite powder of oxidation or non-complete oxidation collects upper solution.
Embodiment 6
A method of graphene oxide solution is prepared, including:
Step 1:At room temperature, the salpeter solution of the concentrated sulfuric acid of 70mL98wt% and 5ml25wt% are mixed, is then delayed while stirring
It is slow that 3.0g graphite powders are added, it is added followed by 1.5g sodium nitrate and 1.6g niter cakes;
Step 2:This mixture is moved into cooling in ice bath, under violent stirring, is slowly added into 9.0g potassium permanganate and 1g
Potassium nitrate;
Step 3:After charging, reaction system is transferred in 40 °C of water-baths, constant temperature stirring is reacted 30 minutes;
Step 4:150mL deionized waters are slowly added to, and water-bath is warming up to 90 °C, are reacted 15 minutes;
Step 5:500mL water is added, the hydrogen peroxide of 15mL30wt% is slowly added to;
Step 6:The mixture of gained filter and washed with the dilute hydrochloric acid of 250mL3.5wt% to remove metal ion,
It is washed with 200mL deionized waters again to remove the acid of remaining;
Step 7:It is diluted in input deionized water after solid filter cake is dried in air, graphite oxide is obtained by being ultrasonically treated
Alkene dispersion liquid;
Step 8:This dispersion liquid is fitted into and is dialysed in bag filter to remove the acid and metal ion of remaining, is changed daily primary
Water is dialysed seven days;
Step 9:Graphene oxide dispersion after dialysis is taken out and is centrifuged under the conditions of 4000 rpms, discards lower layer not
The graphite powder of oxidation or non-complete oxidation collects upper solution.
The graphene oxide solution of the present invention can be applied to field of cell preparation.
Embodiment 7
A method of graphene oxide solution is prepared, including:
Step 1:At room temperature, the salpeter solution of the concentrated sulfuric acid of 70mL98wt% and 5ml25wt% are mixed, is then delayed while stirring
It is slow that 3.0g graphite powders are added, it is added followed by 1.5g sodium nitrate and 1.7g niter cakes;
Step 2:This mixture is moved into cooling in ice bath, under violent stirring, is slowly added into 9.0g potassium permanganate and 1g
Potassium nitrate;
Step 3:After charging, reaction system is transferred in 40 °C of water-baths, constant temperature stirring is reacted 30 minutes;
Step 4:150mL deionized waters are slowly added to, and water-bath is warming up to 90 °C, are reacted 15 minutes;
Step 5:500mL water is added, the hydrogen peroxide of 15mL30wt% is slowly added to;
Step 6:The mixture of gained filter and washed with the dilute hydrochloric acid of 250mL3.5wt% to remove metal ion,
It is washed with 200mL deionized waters again to remove the acid of remaining;
Step 7:It is diluted in input deionized water after solid filter cake is dried in air, graphite oxide is obtained by being ultrasonically treated
Alkene dispersion liquid;
Step 8:This dispersion liquid is fitted into and is dialysed in bag filter to remove the acid and metal ion of remaining, is changed daily primary
Water is dialysed seven days;
Step 9:Graphene oxide dispersion after dialysis is taken out and is centrifuged under the conditions of 4000 rpms, discards lower layer not
The graphite powder of oxidation or non-complete oxidation collects upper solution.
The graphene oxide solution of the present invention can be applied to field of cell preparation.
Embodiment 8
A method of graphene oxide solution is prepared, including:
Step 1:At room temperature, the salpeter solution of the concentrated sulfuric acid of 70mL98wt% and 5ml25wt% are mixed, is then delayed while stirring
It is slow that 3.0g graphite powders are added, it is added followed by 1.5g sodium nitrate and 1.8g niter cakes;
Step 2:This mixture is moved into cooling in ice bath, under violent stirring, is slowly added into 9.0g potassium permanganate and 1g
Potassium nitrate;
Step 3:After charging, reaction system is transferred in 40 °C of water-baths, constant temperature stirring is reacted 30 minutes;
Step 4:150mL deionized waters are slowly added to, and water-bath is warming up to 90 °C, are reacted 15 minutes;
Step 5:500mL water is added, the hydrogen peroxide of 15mL30wt% is slowly added to;
Step 6:The mixture of gained filter and washed with the dilute hydrochloric acid of 250mL3.5wt% to remove metal ion,
It is washed with 200mL deionized waters again to remove the acid of remaining;
Step 7:It is diluted in input deionized water after solid filter cake is dried in air, graphite oxide is obtained by being ultrasonically treated
Alkene dispersion liquid;
Step 8:This dispersion liquid is fitted into and is dialysed in bag filter to remove the acid and metal ion of remaining, is changed daily primary
Water is dialysed seven days;
Step 9:Graphene oxide dispersion after dialysis is taken out and is centrifuged under the conditions of 4000 rpms, discards lower layer not
The graphite powder of oxidation or non-complete oxidation collects upper solution.
The graphene oxide solution of the present invention can be applied to field of cell preparation.
Embodiment 9
A method of graphene oxide solution is prepared, including:
Step 1:At room temperature, the salpeter solution of the concentrated sulfuric acid of 70mL98wt% and 5ml25wt% are mixed, is then delayed while stirring
It is slow that 3.0g graphite powders are added, it is added followed by 1.5g sodium nitrate and 1.9g niter cakes;
Step 2:This mixture is moved into cooling in ice bath, under violent stirring, is slowly added into 9.0g potassium permanganate and 1g
Potassium nitrate;
Step 3:After charging, reaction system is transferred in 40 °C of water-baths, constant temperature stirring is reacted 30 minutes;
Step 4:150mL deionized waters are slowly added to, and water-bath is warming up to 90 °C, are reacted 15 minutes;
Step 5:500mL water is added, the hydrogen peroxide of 15mL30wt% is slowly added to;
Step 6:The mixture of gained filter and washed with the dilute hydrochloric acid of 250mL3.5wt% to remove metal ion,
It is washed with 200mL deionized waters again to remove the acid of remaining;
Step 7:It is diluted in input deionized water after solid filter cake is dried in air, graphite oxide is obtained by being ultrasonically treated
Alkene dispersion liquid;
Step 8:This dispersion liquid is fitted into and is dialysed in bag filter to remove the acid and metal ion of remaining, is changed daily primary
Water is dialysed seven days;
Step 9:Graphene oxide dispersion after dialysis is taken out and is centrifuged under the conditions of 4000 rpms, discards lower layer not
The graphite powder of oxidation or non-complete oxidation collects upper solution.
The graphene oxide solution of the present invention can be applied to field of cell preparation.
Embodiment 10
A method of graphene oxide solution is prepared, including:
Step 1:At room temperature, the salpeter solution of the concentrated sulfuric acid of 70mL98wt% and 5ml25wt% are mixed, is then delayed while stirring
It is slow that 3.0g graphite powders are added, it is added followed by 1.5g sodium nitrate and 2g niter cakes;
Step 2:This mixture is moved into cooling in ice bath, under violent stirring, is slowly added into 9.0g potassium permanganate and 1g
Potassium nitrate;
Step 3:After charging, reaction system is transferred in 40 °C of water-baths, constant temperature stirring is reacted 30 minutes;
Step 4:150mL deionized waters are slowly added to, and water-bath is warming up to 90 °C, are reacted 15 minutes;
Step 5:500mL water is added, the hydrogen peroxide of 15mL30wt% is slowly added to;
Step 6:The mixture of gained filter and washed with the dilute hydrochloric acid of 250mL3.5wt% to remove metal ion,
It is washed with 200mL deionized waters again to remove the acid of remaining;
Step 7:It is diluted in input deionized water after solid filter cake is dried in air, graphite oxide is obtained by being ultrasonically treated
Alkene dispersion liquid;
Step 8:This dispersion liquid is fitted into and is dialysed in bag filter to remove the acid and metal ion of remaining, is changed daily primary
Water is dialysed seven days;
Step 9:Graphene oxide dispersion after dialysis is taken out and is centrifuged under the conditions of 4000 rpms, discards lower layer not
The graphite powder of oxidation or non-complete oxidation collects upper solution.
The graphene oxide solution of the present invention can be applied to field of cell preparation.
Claims (2)
1. a kind of method preparing graphene oxide solution, including:
Step 1:At room temperature, the salpeter solution of the concentrated sulfuric acid of 70mL98wt% and 5ml25wt% are mixed, is then delayed while stirring
It is slow that 3.0g graphite powders are added, it is added followed by 1.5g sodium nitrate and 1.1g niter cakes;
Step 2:This mixture is moved into cooling in ice bath, under violent stirring, is slowly added into 9.0g potassium permanganate and 1g
Potassium nitrate;
Step 3:After charging, reaction system is transferred in 40 °C of water-baths, constant temperature stirring is reacted 30 minutes;
Step 4:150mL deionized waters are slowly added to, and water-bath is warming up to 90 °C, are reacted 15 minutes;
Step 5:500mL water is added, the hydrogen peroxide of 15mL30wt% is slowly added to;
Step 6:The mixture of gained filter and washed with the dilute hydrochloric acid of 250mL3.5wt% to remove metal ion,
It is washed with 200mL deionized waters again to remove the acid of remaining;
Step 7:It is diluted in input deionized water after solid filter cake is dried in air, graphite oxide is obtained by being ultrasonically treated
Alkene dispersion liquid;
Step 8:This dispersion liquid is fitted into and is dialysed in bag filter to remove the acid and metal ion of remaining, is changed daily primary
Water is dialysed seven days;
Step 9:Graphene oxide dispersion after dialysis is taken out and is centrifuged under the conditions of 4000 rpms, discards lower layer not
The graphite powder of oxidation or non-complete oxidation collects upper solution.
2. the graphene oxide solution of the present invention can be applied to field of cell preparation.
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CN201810344209.8A CN108298533A (en) | 2018-04-17 | 2018-04-17 | A method of preparing graphene oxide solution |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109052383A (en) * | 2018-09-05 | 2018-12-21 | 七台河宝泰隆石墨烯新材料有限公司 | A kind of technique of electroosmose process separation graphene oxide |
CN109112692A (en) * | 2018-10-22 | 2019-01-01 | 苏州高研纺织科技有限公司 | A kind of the radar invisible attached Metal Yarns of graphene plating and preparation method |
CN109938038A (en) * | 2019-03-28 | 2019-06-28 | 新冶高科技集团有限公司 | A kind of biology graphene oxide antimicrobial fluid and preparation method thereof |
CN113800806A (en) * | 2021-11-01 | 2021-12-17 | 湖南先锋建材有限公司 | Concrete water reducing agent and production method thereof |
WO2022022050A1 (en) * | 2020-07-27 | 2022-02-03 | 中国港湾工程有限责任公司 | Material for wave wall |
CN115924899A (en) * | 2022-11-19 | 2023-04-07 | 河北麦森钛白粉有限公司 | Preparation method of lithium iron phosphate/graphene oxide composite material |
-
2018
- 2018-04-17 CN CN201810344209.8A patent/CN108298533A/en not_active Withdrawn
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109052383A (en) * | 2018-09-05 | 2018-12-21 | 七台河宝泰隆石墨烯新材料有限公司 | A kind of technique of electroosmose process separation graphene oxide |
CN109112692A (en) * | 2018-10-22 | 2019-01-01 | 苏州高研纺织科技有限公司 | A kind of the radar invisible attached Metal Yarns of graphene plating and preparation method |
CN109938038A (en) * | 2019-03-28 | 2019-06-28 | 新冶高科技集团有限公司 | A kind of biology graphene oxide antimicrobial fluid and preparation method thereof |
CN109938038B (en) * | 2019-03-28 | 2021-06-11 | 新冶高科技集团有限公司 | Graphene oxide antibacterial liquid for biology and preparation method thereof |
WO2022022050A1 (en) * | 2020-07-27 | 2022-02-03 | 中国港湾工程有限责任公司 | Material for wave wall |
CN113800806A (en) * | 2021-11-01 | 2021-12-17 | 湖南先锋建材有限公司 | Concrete water reducing agent and production method thereof |
CN115924899A (en) * | 2022-11-19 | 2023-04-07 | 河北麦森钛白粉有限公司 | Preparation method of lithium iron phosphate/graphene oxide composite material |
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