CN104310385A - Quick green preparation method of single-layer graphene oxide - Google Patents
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Abstract
The invention discloses a quick green preparation method of a single-layer graphene oxide. The quick green preparation method comprises the following steps: 1) mixing graphite with a strong acid at a temperature within the range of -10 to 20 DEG C by stirring for infiltrating for 5 minutes to 1 hour, adding a strong oxidant ferrate and a stabilizer thereof, slowly increasing the temperature to the range of -10 to 80 DEG C and continuously stirring for 0.5 to 24 hours to oxidize and strip graphite flakes; and 2) centrifuging the reaction liquid, removing the strong acid, slowly pouring the muddy product into icy deionized water for diluting, standing, repeatedly washing the precipitate by use of 1mol/L diluted hydrochloric acid and deionized water, and centrifugally separating out the single-layer graphene oxide. The quick green preparation method of the single-layer graphene oxide is simple, safe and controllable in preparation process, low in time and energy consumption, and capable of directly transforming the graphite into the single-layer graphene oxide. More importantly, in the process of preparing the graphene oxide of the method, no polluting halogen and heavy metal oxidant are adopted and no pollution is generated.
Description
Technical field
The present invention relates to field of nanometer material technology, particularly a kind of method of quick Green synthesis single-layer graphene oxide.
Background technology
2004, Univ Manchester UK A.K. Geim teach problem group used mechanically peel method successfully to prepare Graphene, and having overthrown perfect two dimensional crystal structure cannot this judgement of stable existence under non-zero absolute temperature.Then the mechanical property of Graphene excellence, electrical properties, thermal property, optical property are found in succession.Graphene has the theoretical specific surface area of super large, and the excellent properties that has of monolithic layer structure, obtains significant progress and application using Graphene as the carbon-based material of source material in addition.
Oxidation reduction process is prepared Graphene and is considered to most probable and realizes important method prepared by Graphene industrialization.Its intermediate graphene oxide is then the important presoma of Graphene, is the most important intermediate that grapheme material realizes macroscopic view assembling and modification.The macroscopical assembled material fiber, film, aerogel etc. that have realized at present all rely on graphene oxide to prepare.
The existing method preparing graphene oxide mainly contains Brodie, Staudenmaier, Hofmann, Hummers and modified Hummers.These methods are generally generally divided into two kinds according to oxygenant used, based on the Brodie method of Potcrate and the Hummers based on potassium permanganate.But these two kinds of oxygenants not only all easily explode, and speed of reaction is slow.Potcrate easily discharges toxic gas, and potassium permanganate can produce heavy-metal pollution.All these methods all belong to the themes of the times not meeting environmental protection, and therefore the people that arrived of the quick production problem of the green safety of graphene oxide more and more pay attention to.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide a kind of easy a kind of quick green two-step approach to prepare the method for single-layer graphene oxide, the homogeneous dispersion of graphene oxide sheet individual layer prepared by the method, metal ion content is few; The reaction process time period, pollute few, operational safety.
A kind of step of method of quick Green synthesis single-layer graphene oxide is as follows:
1) graphite and strong acid are uniformly mixed at-10-20 DEG C infiltrate 5min-1h, add strong oxidizer ferrate and its stablizer, be slowly warming up to-10-80 DEG C and Keep agitation 0.5-24h, to be oxidized exfoliated graphite layer;
2) reaction solution is centrifugal, discard strong acid, and slowly pour pureed product the deionization dilution with water of ice into, static, the dilute hydrochloric acid of throw out 1mol/L and deionized water are repeatedly cleaned, centrifugation obtains single-layer graphene oxide.
Described strong acid and graphite volume mass ratio are: 40-100ml:1g.The mass ratio of described strong oxidizer, stablizer and graphite is: 4-10g: 0.001-1:1g.The granularity of described graphite is 0.5um-3mm.Described strong acid is sulfuric acid (50%-98%), oleum, chlorsulfonic acid, strong phosphoric acid, concentrated nitric acid, fluosulfonic acid, trifluoromethanesulfonic acid or their mixing acid.Described strong oxidizer is ferrate.Described stablizer is Periodic acid, periodate salt, persulphate, zinc salt, aluminium salt, hypochlorous acid, hypochlorite, chloric acid, oxymuriate, perchloric acid, perchlorate, ortho-phosphoric acid, orthophosphoric acid salt, metaphosphoric acid, metaphosphate, Tripyrophosphoric acid, polyphosphate, boric acid, borate, phosphoric anhydride, ortho-phosphoric acid acid anhydride, metaphosphoric acid acid anhydride, Tripyrophosphoric acid acid anhydride, boron trioxide and their combination thereof.
Preparation process of the present invention is simple and safe controlled, and time consumption and energy consumption is few, by a kind of graphene oxide directly graphite being converted into individual layer.The most important thing is, present method is prepared graphene oxide and is not produced any pollution, and raw material obtains utilizing the most fully, and the graphene oxide contaminative heavy metal ion content of preparation is few.
Accompanying drawing explanation
Fig. 1 is graphene oxide solution (6mg/mL);
Fig. 2 is the scanned picture of graphene oxide;
Fig. 3 is the atomic power picture of graphene oxide.
Embodiment
A kind of step of method of quick Green synthesis single-layer graphene oxide is as follows:
1) graphite and strong acid are uniformly mixed at-10-20 DEG C infiltrate 5min-1h, add strong oxidizer ferrate and its stablizer, be slowly warming up to-10-80 DEG C and Keep agitation 0.5-24h, to be oxidized exfoliated graphite layer;
2) reaction solution is centrifugal, discard strong acid, and slowly pour pureed product the deionization dilution with water of ice into, static, the dilute hydrochloric acid of throw out 1mol/L and deionized water are repeatedly cleaned, centrifugation obtains single-layer graphene oxide.
Described strong acid and graphite volume mass ratio are: 40-100ml:1g.The mass ratio of described strong oxidizer, stablizer and graphite is: 4-10g: 0.001-1:1g.The granularity of described graphite is 0.5-3mm.Described strong acid is sulfuric acid, sulfuric acid (50%-98%), oleum, chlorsulfonic acid, strong phosphoric acid, concentrated nitric acid, fluosulfonic acid, trifluoromethanesulfonic acid or their mixing acid.Described strong oxidizer is ferrate.Described stablizer is Periodic acid, periodate salt, persulphate, zinc salt, aluminium salt, hypochlorous acid, hypochlorite, chloric acid, oxymuriate, perchloric acid, perchlorate, ortho-phosphoric acid, orthophosphoric acid salt, metaphosphoric acid, metaphosphate, Tripyrophosphoric acid, polyphosphate, boric acid, borate, phosphoric anhydride, ortho-phosphoric acid acid anhydride, metaphosphoric acid acid anhydride, Tripyrophosphoric acid acid anhydride, boron trioxide and their combination thereof.
Embodiment 1
The graphite of granularity at 0.5 μm is uniformly mixed infiltrates 0.5h with the vitriol oil of being fuming at-10 DEG C, adds potassium ferrate and Potassium Persulphate.Subsequently reaction solution is risen to 0 DEG C of reaction 1h.After completion of the reaction, by centrifugal for reaction solution to discard strong acid.Bottom sediment thing is slowly poured into the deionization dilution with water of ice, static for some time, the dilute hydrochloric acid of throw out 1mol/L and deionized water are repeatedly cleaned, centrifugation obtains single-layer graphene oxide.In reaction process, the ratio of strong acid and graphite is 40ml:1g, potassium ferrate, and the ratio of Potassium Persulphate and graphite is 4g:0.01g:1g.
Embodiment 2
Granularity is uniformly mixed at the graphite of 40 μm and sulfuric acid (50%) at-10 DEG C and infiltrates 0.5h, add potassium ferrate and Periodic acid.Subsequently reaction solution is risen to 0 DEG C of reaction 1h.After completion of the reaction, by centrifugal for reaction solution to discard strong acid.Bottom sediment thing is slowly poured into the deionization dilution with water of ice, static for some time, the dilute hydrochloric acid of throw out 1mol/L and deionized water are repeatedly cleaned, centrifugation obtains single-layer graphene oxide.In reaction process, the ratio of strong acid and graphite is 50ml:1g, potassium ferrate, and the ratio of Periodic acid and graphite is 6g:0.001g:1g.
By accompanying drawing 1, the graphene oxide of preparation has good solubility, and defines liquid crystal.Can be found out by accompanying drawing 2, SEM picture, prepared graphene oxide thickness distribution is even, and pleated portions divides explanation lamella to have certain flexibility; As can be seen from accompanying drawing 3 by AFM, prepared graphene oxide thickness at about 1.1nm, namely individual layer.
Embodiment 3
Granularity is uniformly mixed at the graphite of 40 μm and sulfuric acid (98%) at-10 DEG C and infiltrates 0.5h, add potassium ferrate and Periodic acid.Subsequently reaction solution is risen to 0 DEG C of reaction 1h.After completion of the reaction, by centrifugal for reaction solution to discard strong acid.Bottom sediment thing is slowly poured into the deionization dilution with water of ice, static for some time, the dilute hydrochloric acid of throw out 1mol/L and deionized water are repeatedly cleaned, centrifugation obtains single-layer graphene oxide.In reaction process, the ratio of strong acid and graphite is 50ml:1g, potassium ferrate, and the ratio of Periodic acid and graphite is 6g:0.001g:1g.
Embodiment 4
Granularity is uniformly mixed at the graphite of 40 μm and strong phosphoric acid at 0 DEG C and infiltrates 1h, add potassium ferrate and boric acid.Subsequently reaction solution is risen to 20 DEG C of reaction 2h.After completion of the reaction, by centrifugal for reaction solution to discard strong acid.Bottom sediment thing is slowly poured into the deionization dilution with water of ice, static for some time, the dilute hydrochloric acid of throw out 1mol/L and deionized water are repeatedly cleaned, centrifugation obtains single-layer graphene oxide.In reaction process, the ratio of strong acid and graphite is 60ml:1g, potassium ferrate, and the ratio of Potassium Persulphate and boric acid is 10g:0.1g:1g.
Embodiment 5
Granularity is uniformly mixed at the graphite of 100 μm and the vitriol oil and strong phosphoric acid at 20 DEG C and infiltrates 0.1h, add potassium ferrate and zinc chloride.Subsequently reaction solution is risen to 40 DEG C of reaction 4h.After completion of the reaction, by centrifugal for reaction solution to discard strong acid.Bottom sediment thing is slowly poured into the deionization dilution with water of ice, static for some time, the dilute hydrochloric acid of throw out 1mol/L and deionized water are repeatedly cleaned, centrifugation obtains single-layer graphene oxide.In reaction process, the ratio of the vitriol oil, strong phosphoric acid and graphite is 80ml:20ml:1g, potassium ferrate, and the ratio of zinc chloride and graphite is 7g:0.4g:1g.
Embodiment 6
Granularity is uniformly mixed at the graphite of 500 μm and oleum and strong phosphoric acid at 20 DEG C and infiltrates 0.1h, add potassium ferrate and perchloric acid.Subsequently reaction solution is risen to 40 DEG C of reaction 4h.After completion of the reaction, by centrifugal for reaction solution to discard strong acid.Bottom sediment thing is slowly poured into the deionization dilution with water of ice, static for some time, the dilute hydrochloric acid of throw out 1mol/L and deionized water are repeatedly cleaned, centrifugation obtains single-layer graphene oxide.In reaction process, the ratio of strong acid and graphite is 90ml:1g, potassium ferrate, and the ratio of perchloric acid and graphite is 9g:1g:1g.
Embodiment 7
Granularity is uniformly mixed at the graphite of 1mm and oleum at 20 DEG C and infiltrates 0.5h, add potassium ferrate and clorox.Subsequently reaction solution is risen to 60 DEG C of reaction 6h.After completion of the reaction, by centrifugal for reaction solution to discard strong acid.Bottom sediment thing is slowly poured into the deionization dilution with water of ice, static for some time, the dilute hydrochloric acid of throw out 1mol/L and deionized water are repeatedly cleaned, centrifugation obtains single-layer graphene oxide.In reaction process, the ratio of strong acid and graphite is 100ml:1g, potassium ferrate, and the ratio of sodium perchlorate and graphite is 10g:1g:1g.
Embodiment 8
Granularity is uniformly mixed at the graphite of 2mm and the vitriol oil at 20 DEG C and infiltrates 1h, add potassium ferrate and metaphosphoric acid acid anhydride.Subsequently reaction solution is risen to 60 DEG C of reaction 6h.After completion of the reaction, by centrifugal for reaction solution to discard strong acid.Bottom sediment thing is slowly poured into the deionization dilution with water of ice, static for some time, the dilute hydrochloric acid of throw out 1mol/L and deionized water are repeatedly cleaned, centrifugation obtains single-layer graphene oxide.In reaction process, the ratio of strong acid and graphite is 100ml:1g, potassium ferrate, and the ratio of metaphosphoric acid acid anhydride and graphite is 10g:0.3g:1g.
Embodiment 9
Granularity is uniformly mixed at the graphite of 3mm and the vitriol oil at 20 DEG C and infiltrates 1h, add potassium ferrate and sodium chlorate.Subsequently reaction solution is risen to 60 DEG C of reaction 6h.After completion of the reaction, by centrifugal for reaction solution to discard strong acid.Bottom sediment thing is slowly poured into the deionization dilution with water of ice, static for some time, the dilute hydrochloric acid of throw out 1mol/L and deionized water are repeatedly cleaned, centrifugation obtains single-layer graphene oxide.In reaction process, the ratio of strong acid and graphite is 100ml:1g, potassium ferrate, and the ratio of sodium chlorate and graphite is 8g:0.6g:1g.
Embodiment 10
Granularity is uniformly mixed at the graphite of 3mm and the vitriol oil at 20 DEG C and infiltrates 1h, add potassium ferrate and metaphosphoric acid acid anhydride.Subsequently reaction solution is risen to 60 DEG C of reaction 6h.After completion of the reaction, by centrifugal for reaction solution to discard strong acid.Bottom sediment thing is slowly poured into the deionization dilution with water of ice, static for some time, the dilute hydrochloric acid of throw out 1mol/L and deionized water are repeatedly cleaned, centrifugation obtains single-layer graphene oxide.In reaction process, the ratio of strong acid and graphite is 100ml:1g, potassium ferrate, and the ratio of potassium metaphosphate and graphite is 6g:1g:1g.
Embodiment 11
Granularity is uniformly mixed at the graphite of 3mm and the vitriol oil at 20 DEG C and infiltrates 1h, add potassium ferrate and metaphosphoric acid acid anhydride.Subsequently reaction solution is risen to 60 DEG C of reaction 6h.After completion of the reaction, by centrifugal for reaction solution to discard strong acid.Bottom sediment thing is slowly poured into the deionization dilution with water of ice, static for some time, the dilute hydrochloric acid of throw out 1mol/L and deionized water are repeatedly cleaned, centrifugation obtains single-layer graphene oxide.In reaction process, the ratio of strong acid and graphite is 100ml:1g, potassium ferrate, potassium borate, and the ratio of sodium phosphate and graphite is 10g:0.4g:0.2g:1g.
Above-described embodiment is used for explaining and the present invention is described, instead of limits the invention, and in the protection domain of spirit of the present invention and claim, any amendment make the present invention and change, all fall into protection scope of the present invention.
Claims (7)
1. a method for quick Green synthesis single-layer graphene oxide, is characterized in that: its step is as follows:
1) graphite and strong acid are uniformly mixed at-10-20 DEG C infiltrate 5min-1h, add strong oxidizer ferrate and its stablizer, be slowly warming up to-10-80 DEG C and Keep agitation 0.5-24h, to be oxidized exfoliated graphite layer;
2) reaction solution is centrifugal, discard strong acid, and slowly pour pureed product the deionization dilution with water of ice into, static, the dilute hydrochloric acid of throw out 1mol/L and deionized water are repeatedly cleaned, centrifugation obtains single-layer graphene oxide.
2. the method for a kind of quick Green synthesis single-layer graphene oxide as claimed in claim 1, is characterized in that: described strong acid and graphite volume mass ratio are: 40-100ml:1g.
3. the method for a kind of quick Green synthesis single-layer graphene oxide as claimed in claim 1, is characterized in that: the mass ratio of described strong oxidizer, stablizer and graphite is: 4-10g: 0.001-1:1g.
4. the method for a kind of quick Green synthesis single-layer graphene oxide according to claim 1, is characterized in that, the granularity of described graphite is 0.5um-3mm.
5. the method for a kind of quick Green synthesis single-layer graphene oxide according to claim 1, it is characterized in that, described strong acid is sulfuric acid, sulfuric acid (50%-98%), oleum, chlorsulfonic acid, strong phosphoric acid, concentrated nitric acid, fluosulfonic acid, trifluoromethanesulfonic acid or their mixing acid.
6. the method for a kind of quick Green synthesis single-layer graphene oxide according to claim 1, it is characterized in that, described strong oxidizer is ferrate.
7. the method for a kind of quick Green synthesis single-layer graphene oxide according to claim 1, it is characterized in that, described stablizer is Periodic acid, periodate salt, persulphate, zinc salt, aluminium salt, hypochlorous acid, hypochlorite, chloric acid, oxymuriate, perchloric acid, perchlorate, ortho-phosphoric acid, orthophosphoric acid salt, metaphosphoric acid, metaphosphate, Tripyrophosphoric acid, polyphosphate, boric acid, borate, phosphoric anhydride, ortho-phosphoric acid acid anhydride, metaphosphoric acid acid anhydride, Tripyrophosphoric acid acid anhydride, boron trioxide and their combination thereof.
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| PCT/CN2015/070511 WO2016054877A1 (en) | 2014-10-09 | 2015-01-12 | Rapid and environmentally-friendly method for preparing single-layer graphene oxide |
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| CN105176067A (en) * | 2015-10-22 | 2015-12-23 | 江南大学 | Preparation method of single-layer graphene oxide modified waterborne polyurethane composite material |
| CN105233706A (en) * | 2015-09-23 | 2016-01-13 | 三达膜科技（厦门）有限公司 | Oxidized graphene metal/metallic oxide nanoparticle modified hollow fiber ultrafiltration membrane, and preparation method thereof |
| CN105752963A (en) * | 2016-01-25 | 2016-07-13 | 浙江碳谷上希材料科技有限公司 | Foldable electrothermal film device based on graphene |
| CN106082147A (en) * | 2016-05-31 | 2016-11-09 | 山东大学 | A kind of method that boron nitride nanosheet is prepared in stable liquid phase chemical stripping |
| CN107140632A (en) * | 2017-06-20 | 2017-09-08 | 上海大学 | A kind of preparation method of the large-size graphene oxide sheet layer of high mechanical strength |
| CN107226469A (en) * | 2017-08-03 | 2017-10-03 | 山东金城石墨烯科技有限公司 | A kind of method that one-step method prepares graphene oxide |
| CN107585761A (en) * | 2017-10-13 | 2018-01-16 | 南京旭羽睿材料科技有限公司 | A kind of expanded graphite alkene preparation method |
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Patent Citations (2)
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| CN102803135A (en) * | 2009-05-22 | 2012-11-28 | 威廉马歇莱思大学 | Highly Oxidized Graphene Oxide And Methods For Production Thereof |
| CN103145121A (en) * | 2013-03-19 | 2013-06-12 | 苏州格瑞丰纳米科技有限公司 | Preparation method of thin-layer graphene oxide material |
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| CN105233706A (en) * | 2015-09-23 | 2016-01-13 | 三达膜科技（厦门）有限公司 | Oxidized graphene metal/metallic oxide nanoparticle modified hollow fiber ultrafiltration membrane, and preparation method thereof |
| CN105176067A (en) * | 2015-10-22 | 2015-12-23 | 江南大学 | Preparation method of single-layer graphene oxide modified waterborne polyurethane composite material |
| CN105176067B (en) * | 2015-10-22 | 2018-03-30 | 江南大学 | A kind of preparation method of single-layer graphene oxide modified aqueous polyurethane composite |
| CN105752963A (en) * | 2016-01-25 | 2016-07-13 | 浙江碳谷上希材料科技有限公司 | Foldable electrothermal film device based on graphene |
| CN105752963B (en) * | 2016-01-25 | 2017-10-31 | 浙江碳谷上希材料科技有限公司 | A kind of foldable electrothermal film device based on graphene |
| CN106082147A (en) * | 2016-05-31 | 2016-11-09 | 山东大学 | A kind of method that boron nitride nanosheet is prepared in stable liquid phase chemical stripping |
| CN106082147B (en) * | 2016-05-31 | 2018-06-05 | 山东大学 | The method that a kind of liquid phase chemical stripping of stabilization prepares boron nitride nanosheet |
| CN107140632A (en) * | 2017-06-20 | 2017-09-08 | 上海大学 | A kind of preparation method of the large-size graphene oxide sheet layer of high mechanical strength |
| CN107226469A (en) * | 2017-08-03 | 2017-10-03 | 山东金城石墨烯科技有限公司 | A kind of method that one-step method prepares graphene oxide |
| CN107585761A (en) * | 2017-10-13 | 2018-01-16 | 南京旭羽睿材料科技有限公司 | A kind of expanded graphite alkene preparation method |
| KR20200018019A (en) * | 2018-08-10 | 2020-02-19 | 한국전력공사 | Method for low defective graphene oxide using antioxidant and graphene oxide thereby |
| KR102550123B1 (en) | 2018-08-10 | 2023-07-03 | 한국전력공사 | Method for low defective graphene oxide using antioxidant and graphene oxide thereby |
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