CN106744908A - Improve the method that Hummers methods prepare graphene oxide - Google Patents
Improve the method that Hummers methods prepare graphene oxide Download PDFInfo
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- CN106744908A CN106744908A CN201611043368.1A CN201611043368A CN106744908A CN 106744908 A CN106744908 A CN 106744908A CN 201611043368 A CN201611043368 A CN 201611043368A CN 106744908 A CN106744908 A CN 106744908A
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- mixed liquor
- graphene oxide
- hummers methods
- prepare graphene
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
Abstract
The present invention relates to industrial water and waste water technology field, and in particular to a kind of method that improvement Hummers methods prepare graphene oxide.The Hummers methods method for preparing graphene oxide is improved, graphite powder is put into, in three-neck flask, and add mixed liquor；Under condition of ice bath, KMnO is added4, by mixed liquor, stirring；To react after the mixed liquor that obtains is cooled to room temperature, be poured on spend ion water making into ice cube on, about 3mLH is added under agitation2O2；After mixture is filtered, removal of residue is removed 5 times in centrifuge washing with HCl；Products therefrom is loaded into bag filter, after dialysing 3 weeks, vacuum freeze drier drying to constant weight is placed in, the GO powder of brown is obtained；Weigh 1gGO powder to be scattered in deionized water and constant volume, ultrasound obtains GO dispersion liquids.The present invention can prepare GO, and GO contains the oxygen-containing functional groups such as carboxyl, hydroxyl and epoxy radicals, and C, O mass ratio reach 2.0, and thickness is about 1.0nm, and interlamellar spacing is about 0.97nm.
Description
Technical field
The present invention relates to industrial water and waste water technology field, and in particular to one kind improves Hummers methods and prepares oxidation stone
The method of black alkene.
Background technology
Graphene be one kind by carbon atom with sp2Hybridized orbit composition is in the two-dimentional material of cellular regular hexagon layer structure
Material, only 1 carbon atom (0.334nm) thickness.Graphene has huge specific surface area, and theoretical value is up to 2620m2/ g, therefore quilt
It is considered a kind of adsorbent with applications well prospect.The graphene oxide of one of Graphene race material important member, except guarantor
Hold outside the huge specific surface area of Graphene, introduced on six-membered carbon ring a large amount of such as electronegativity such as epoxy radicals, hydroxyl and carboxyls
Oxygen-containing functional group, by Electrostatic Absorption can effectively Liquidity limit, therefore can be used for the absorption to metal cation.
Relative to traditional carbon adsorbing material, the adsorption capacity of GO has significant advantage.Yang etc. analyzes GO to Cu2+Absorption
Meet Langmuir models, when pH value is 5.0, GO is to Cu2+Adsorbance reach 46.6mg/g, far above CNT
4 ~ the 5mg/g of 28.5mg/g and activated carbon.Ren etc. compared for GO, activated carbon and multi-walled carbon nano-tubes to Cu2+Adsorption capacity obtain
Go out, when pH value is 5.95, to Cu2+Maximal absorptive capacity be ordered as GO ﹥ activated carbon ﹥ multi-walled carbon nano-tubes.Zhao etc. synthesizes
About 2 ~ 3 layers of GO, obtains GO to Pb2+、Cd2+、Co2+And U6+Maximal absorptive capacity be respectively 842,106.3,68.2 and 97.5mg/
G, far above other nano adsorbers.It is to be with Hummers methods in most researchs on GO adsorbing metal ions
Preparation method.But, in preparation process, because using NaNO3As one of oxidant, NO can be produced2And N2O4Deng murder by poisoning gas
Body, and remnants Na+More difficult removal, may produce influence to GO adsorbing metals cation.
The content of the invention
The present invention is directed to propose a kind of method that improvement Hummers methods prepare graphene oxide.
Technical program of the present invention lies in：
The method that Hummers methods prepare graphene oxide is improved, is comprised the following steps：
1st step, in putting 3 ~ 4g graphite powders into 500mL three-neck flasks, and adds H2SO4With H3PO4Mixed liquor；
2nd step, under condition of ice bath, adds 18gKMnO4, 10 ~ 12h is stirred at mixed liquor is maintained at into 50 ~ 60 DEG C；
3rd step, will react after the mixed liquor that obtains is cooled to room temperature, be poured on the ice cube being made of 350 ~ 400mL deionized waters,
About 3mLH is added under agitation2O2, now mixed liquor glassy yellow is transformed into by atropurpureus；After mixture is filtered, existed with HCl
Centrifuge washing removes removal of residue 5 times under 10000 ~ 12000r/min；Products therefrom is loaded into bag filter, after dialysing 3 weeks, is placed in true
The drying of vacuum freecing-dry machine obtains the GO powder of brown to constant weight；
4th step, weighs 1gGO powder and is scattered in deionized water and is settled to 1000mL, ultrasound, obtains mass concentration for 1mg/
The GO dispersion liquids of mL.
Described H2SO4With H3PO4Mixed liquor in, H2SO4In volume be 360mL, H3PO4Volume be 40mL.
The described dry time is 45 ~ 48h.
The time of described dry ultrasound is 4h, and the power of ultrasound is 300W.
Described H2SO4Volume fraction be 98%, H3PO4Volume fraction be 85%, H2O2Volume fraction be 30%.
The technical effects of the invention are that：
The present invention can prepare GO using Hummers methods are improved, and GO contains the oxygen-containing functional groups such as carboxyl, hydroxyl and epoxy radicals, C, O
Mass ratio reaches 2.0, and thickness is about 1.0nm, and interlamellar spacing is about 0.97nm.
Specific embodiment
The method that Hummers methods prepare graphene oxide is improved, is comprised the following steps：
Embodiment 1
1st step, in putting 3g graphite powders into 500mL three-neck flasks, and adds H2SO4With H3PO4Mixed liquor；
2nd step, under condition of ice bath, adds 18gKMnO4, mixed liquor is maintained at 50 DEG C and stirs 10h；
3rd step, will react after the mixed liquor that obtains is cooled to room temperature, be poured on the ice cube being made of 350mL deionized waters, stir
Mix lower addition about H2O2, now mixed liquor glassy yellow is transformed into by atropurpureus；After mixture is filtered, with HCl in 10000r/min
Lower centrifuge washing removes removal of residue 5 times；Products therefrom is loaded into bag filter, after dialysing 3 weeks, vacuum freeze drier drying is placed in
To constant weight, the GO powder of brown is obtained；
4th step, weighs 1gGO powder and is scattered in deionized water and is settled to 1000mL, ultrasound, obtains mass concentration for 1mg/
The GO dispersion liquids of mL.
Wherein, described H2SO4With H3PO4Mixed liquor in, H2SO4In volume be 360mL, H3PO4Volume be
40mL.The described dry time is 45h.The time of described dry ultrasound is 4h, and the power of ultrasound is 300W.Described
H2SO4Volume fraction be 98%, H3PO4Volume fraction be 85%, H2O2Volume fraction be 30%.
Embodiment 2
1st step, in putting 4g graphite powders into 500mL three-neck flasks, and adds H2SO4With H3PO4Mixed liquor；
2nd step, under condition of ice bath, adds 18gKMnO4, mixed liquor is maintained at 60 DEG C and stirs 12h；
3rd step, will react after the mixed liquor that obtains is cooled to room temperature, be poured on the ice cube being made of 400mL deionized waters, stir
Mix lower addition about 3mL H2O2, now mixed liquor glassy yellow is transformed into by atropurpureus；After mixture is filtered, existed with HCl
Centrifuge washing removes removal of residue 5 times under 12000r/min；Products therefrom is loaded into bag filter, after dialysing 3 weeks, vacuum refrigeration is placed in
Drying machine drying obtains the GO powder of brown to constant weight；
4th step, weighs 1gGO powder and is scattered in deionized water and is settled to 1000mL, ultrasound, obtains mass concentration for 1mg/
The GO dispersion liquids of mL.
Wherein, described H2SO4With H3PO4Mixed liquor in, H2SO4In volume be 360mL, H3PO4Volume be
40mL.The described dry time is 48h.The time of described dry ultrasound is 4h, and the power of ultrasound is 300W.Described
H2SO4Volume fraction be 98%, H3PO4Volume fraction be 85%, H2O2Volume fraction be 30%.
Claims (5)
1. the method that Hummers methods prepare graphene oxide is improved, it is characterised in that：Comprise the following steps：
1st step, in putting 3 ~ 4g graphite powders into 500mL three-neck flasks, and adds H2SO4With H3PO4Mixed liquor；
2nd step, under condition of ice bath, adds 18gKMnO4, 10 ~ 12h is stirred at mixed liquor is maintained at into 50 ~ 60 DEG C；
3rd step, will react after the mixed liquor that obtains is cooled to room temperature, be poured on the ice cube being made of 350 ~ 400mL deionized waters,
About 3mLH is added under agitation2O2, now mixed liquor glassy yellow is transformed into by atropurpureus；After mixture is filtered, existed with HCl
Centrifuge washing removes removal of residue 5 times under 10000 ~ 12000r/min；Products therefrom is loaded into bag filter, after dialysing 3 weeks, is placed in true
The drying of vacuum freecing-dry machine obtains the GO powder of brown to constant weight；
4th step, weighs 1gGO powder and is scattered in deionized water and is settled to 1000mL, ultrasound, obtains mass concentration for 1mg/
The GO dispersion liquids of mL.
2. the method that improvement Hummers methods according to claim 1 prepare graphene oxide, it is characterised in that：Described
H2SO4With H3PO4Mixed liquor in, H2SO4In volume be 360mL, H3PO4Volume be 40mL.
3. the method that improvement Hummers methods according to claim 1 prepare graphene oxide, it is characterised in that：Described
The dry time is 45 ~ 48h.
4. the method that improvement Hummers methods according to claim 1 prepare graphene oxide, it is characterised in that：Described
The time of dry ultrasound is 4h, and the power of ultrasound is 300W.
5. the method that improvement Hummers methods according to claim 1 prepare graphene oxide, it is characterised in that：Described
H2SO4Volume fraction be 98%, H3PO4Volume fraction be 85%, H2O2Volume fraction be 30%.
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| CN201611043368.1A CN106744908A (en) | 2016-11-24 | 2016-11-24 | Improve the method that Hummers methods prepare graphene oxide |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107226468A (en) * | 2017-07-06 | 2017-10-03 | 四川农业大学 | A kind of improvement Hummers methods prepare the method and its obtained graphene oxide of graphene oxide |
| CN109133040A (en) * | 2018-08-07 | 2019-01-04 | 北京科技大学 | A kind of preparation method of the adjustable graphene aerogel of pore-size |
| CN114479708A (en) * | 2022-03-16 | 2022-05-13 | 常州宏巨电子科技有限公司 | Preparation method of epoxy resin-based heat-conducting heat-resistant electric-conducting adhesive film |
| CN115355444A (en) * | 2022-09-08 | 2022-11-18 | 燕山大学 | Method for efficiently storing methane gas |
-
2016
- 2016-11-24 CN CN201611043368.1A patent/CN106744908A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107226468A (en) * | 2017-07-06 | 2017-10-03 | 四川农业大学 | A kind of improvement Hummers methods prepare the method and its obtained graphene oxide of graphene oxide |
| CN107226468B (en) * | 2017-07-06 | 2019-04-30 | 四川农业大学 | It is a kind of improvement Hummers method prepare graphene oxide method and its graphene oxide obtained |
| CN109133040A (en) * | 2018-08-07 | 2019-01-04 | 北京科技大学 | A kind of preparation method of the adjustable graphene aerogel of pore-size |
| CN109133040B (en) * | 2018-08-07 | 2020-05-12 | 北京科技大学 | Preparation method of graphene aerogel with adjustable pore size |
| CN114479708A (en) * | 2022-03-16 | 2022-05-13 | 常州宏巨电子科技有限公司 | Preparation method of epoxy resin-based heat-conducting heat-resistant electric-conducting adhesive film |
| CN115355444A (en) * | 2022-09-08 | 2022-11-18 | 燕山大学 | Method for efficiently storing methane gas |
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