CN108298533A - A method of preparing graphene oxide solution - Google Patents

A method of preparing graphene oxide solution Download PDF

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Publication number
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
graphene oxide
added
slowly added
stirring
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程桂平
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2204/00Structure or properties of graphene
    • C01B2204/20Graphene characterized by its properties
    • C01B2204/22Electronic properties

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  • Battery Electrode And Active Subsutance (AREA)

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

A method of preparing graphene oxide solution
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.
CN201810344209.8A 2018-04-17 2018-04-17 A method of preparing graphene oxide solution Withdrawn CN108298533A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
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
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

Cited By (7)

* Cited by examiner, † Cited by third party
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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