CN106744822A - The go back original reagent and restoring method of graphene oxide - Google Patents
The go back original reagent and restoring method of graphene oxide Download PDFInfo
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- CN106744822A CN106744822A CN201510792288.5A CN201510792288A CN106744822A CN 106744822 A CN106744822 A CN 106744822A CN 201510792288 A CN201510792288 A CN 201510792288A CN 106744822 A CN106744822 A CN 106744822A
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Abstract
It is NaHSO the present invention relates to a kind of go back original reagent of graphene oxide3, Na2S‧9H2O, Na2S2O3, SOCl2Or SO2The aqueous solution.Additionally relate to the restoring method using the graphene oxide of this reducing agent, 100mg graphene oxide powders are dispersed in the water of 100ml the graphene oxide water solution for being made 1mg/mL, 1 2h of ultrasonic cleaning machine ultrasound obtains solution, ultrasonic power is 90 110w, add the reducing agent of 1 3mmol, mixed solution stirs 2 3h under being warmed up to 90 100 °C, then filter and repeatedly washed with deionized water, reduced graphene of the product by acquisition black powder after freeze-drying process.Used as the reagent for reducing GO, these reducing agents can efficiently reduce GO to a series of sulfur-containing compounds of Bian, while having cheap feature, can substantially reduce production cost in the present invention.
Description
Technical field
The invention belongs to technical field of polymer materials, and in particular to the go back original reagent and restoring method of a kind of graphene oxide.
Background technology
It is an important synthesis path by chemical oxidation and then reduction in the dilute preparation method of graphite.Although the method that solvothermal deoxidation prepares reduced graphene can obtain scattered graphite weak solution, reducing degree is not very high, and oxygen content is still excessive, and electrical conductance also has much room for improvement.And it is then relatively more common by chemical reduction method to prepare the dilute work of graphite in solution, used reducing agent includes hydration hydrazine and its derivative, amino acid, NaBH cruel to benzene two in current document report4, NaOH and vitamin etc..Additionally, also having been reported that using the method for electrochemical reduction.In the dilute reducing agent of graphite oxide, hydration callosity and its derivative are most widely used because of its efficient reducing power.Yet with introducing N doping in reduction process, it is difficult to which the graphite for obtaining high-purity and high conduction performance is dilute.Additionally, the chemicals of hydration callosity or severe toxicity and explosive, therefore many problems are faced in large-scale use.Another strong reductant NaBH4Although also can more efficiently reduce GO, but because its unstable, easy hydrolysis, cause the reducing agent in use under efficiency.Remaining reducing agent such as NaOH, then reduction efficiency is relatively low extremely to wait benzene two reagent.Therefore it is that chemical method prepares a dilute important step of reduction graphite, nearest Paredes et al. report vitamin C for the reduction of GO to find efficient reducing agent, can reach the reduction effect close to hydration callosity；New reducing agent especially cheap chemicals is found, is an important thinking to reach the purpose of reduction GO in water phase.
The content of the invention
Regarding to the issue above, the present invention is intended to provide the go back original reagent and restoring method of a kind of graphene oxide.
A kind of go back original reagent of graphene oxide, is NaHSO3, Na2S‧9H2O, Na2S2O3, SOCl2Or SO2The aqueous solution.
A kind of restoring method of graphene oxide, 100 mg graphene oxide powders are dispersed in the water of 100ml the graphene oxide water solution for being made 1mg/mL, ultrasonic cleaning machine ultrasound 1-2h obtains solution, ultrasonic power is 90-110w, add the reducing agent of 1-3 mmol, mixed solution stirs 2-3h under being warmed up to 90-100 °C, then filter and repeatedly washed with deionized water, reduced graphene of the product by acquisition black powder after freeze-drying process.
Used as the reagent for reducing GO, these reducing agents can efficiently reduce GO to a series of sulfur-containing compounds of Bian, while having cheap feature, can substantially reduce production cost in the present invention.
Specific embodiment
The present invention is described in further details with reference to specific embodiment.
Embodiment 1
A kind of restoring method of graphene oxide, 100 mg graphene oxide powders are dispersed in the water of 100ml the graphene oxide water solution for being made 1mg/mL, and ultrasonic cleaning machine ultrasound 1h obtains solution, and ultrasonic power is 90w, adds the NaHSO of 2 mmol3, mixed solution stirs 2h under being warmed up to 90 °C, then filter and repeatedly washed with deionized water, and product is by obtaining the reduced graphene of black powder after freeze-drying process.
Embodiment 2
A kind of restoring method of graphene oxide, 100 mg graphene oxide powders are dispersed in the water of 100ml the graphene oxide water solution for being made 1mg/mL, and 1.5 h of ultrasonic cleaning machine ultrasound obtain solution, and ultrasonic power is 100w, add the Na of 1 mmol2S‧9H2O, mixed solution stirs 2.5h under being warmed up to 95 °C, then filter and repeatedly washed with deionized water, reduced graphene of the product by acquisition black powder after freeze-drying process.
Embodiment 3
A kind of restoring method of graphene oxide, 100 mg graphene oxide powders are dispersed in the water of 100ml the graphene oxide water solution for being made 1mg/mL, and ultrasonic cleaning machine ultrasound 1.5h obtains solution, and ultrasonic power is 95w, adds the Na of 3 mmol2S2O3, mixed solution stirs 2h under being warmed up to 90 °C, then filter and repeatedly washed with deionized water, and product is by obtaining the reduced graphene of black powder after freeze-drying process.
Embodiment 4
A kind of restoring method of graphene oxide, 100 mg graphene oxide powders are dispersed in the water of 100ml the graphene oxide water solution for being made 1mg/mL, and ultrasonic cleaning machine ultrasound 1h obtains solution, and ultrasonic power is 105w, adds the SOCl of 2.5 mmol2, mixed solution stirs 3h under being warmed up to 90 °C, then filter and repeatedly washed with deionized water, and product is by obtaining the reduced graphene of black powder after freeze-drying process.
Embodiment 5
A kind of restoring method of graphene oxide, 100 mg graphene oxide powders are dispersed in the water of 100ml the graphene oxide water solution for being made 1mg/mL, and ultrasonic cleaning machine ultrasound 2h obtains solution, and ultrasonic power is 110w, adds the SO of 1.5 mmol2, mixed solution stirs 2.5h under being warmed up to 100 °C, then filter and repeatedly washed with deionized water, and product is by obtaining the reduced graphene of black powder after freeze-drying process.
Claims (2)
1. a kind of go back original reagent of graphene oxide, it is characterised in that be NaHSO3, Na2S‧9H2O, Na2S2O3, SOCl2Or SO2The aqueous solution.
2. the restoring method of the graphene oxide of the go back original reagent described in a kind of use claim 1, it is characterized in that, 100 mg graphene oxide powders are dispersed in the water of 100ml the graphene oxide water solution for being made 1mg/mL, ultrasonic cleaning machine ultrasound 1-2h obtains solution, ultrasonic power is 90-110w, add the reducing agent of 1-3 mmol, mixed solution stirs 2-3h under being warmed up to 90-100 °C, then filter and repeatedly washed with deionized water, reduced graphene of the product by acquisition black powder after freeze-drying process.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510792288.5A CN106744822A (en) | 2015-11-18 | 2015-11-18 | The go back original reagent and restoring method of graphene oxide |
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| CN201510792288.5A CN106744822A (en) | 2015-11-18 | 2015-11-18 | The go back original reagent and restoring method of graphene oxide |
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| CN106744822A true CN106744822A (en) | 2017-05-31 |
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| CN201510792288.5A Pending CN106744822A (en) | 2015-11-18 | 2015-11-18 | The go back original reagent and restoring method of graphene oxide |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110729133A (en) * | 2019-11-13 | 2020-01-24 | 广西科学院应用物理研究所 | Preparation method of polypyrrole-polycaprolactone-graphene ternary nanocomposite |
| CN115285977A (en) * | 2022-06-24 | 2022-11-04 | 深圳材启新材料有限公司 | Method for preparing graphene from graphene oxide |
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2015
- 2015-11-18 CN CN201510792288.5A patent/CN106744822A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110729133A (en) * | 2019-11-13 | 2020-01-24 | 广西科学院应用物理研究所 | Preparation method of polypyrrole-polycaprolactone-graphene ternary nanocomposite |
| CN110729133B (en) * | 2019-11-13 | 2021-08-27 | 广西科学院应用物理研究所 | Preparation method of polypyrrole-polycaprolactone-graphene ternary nanocomposite |
| CN115285977A (en) * | 2022-06-24 | 2022-11-04 | 深圳材启新材料有限公司 | Method for preparing graphene from graphene oxide |
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Application publication date: 20170531 |