CN102275897A - Method for diluting concentrated sulfuric acid by using mixture of ice and water during graphite oxide preparation - Google Patents
Method for diluting concentrated sulfuric acid by using mixture of ice and water during graphite oxide preparation Download PDFInfo
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- CN102275897A CN102275897A CN 201110143062 CN201110143062A CN102275897A CN 102275897 A CN102275897 A CN 102275897A CN 201110143062 CN201110143062 CN 201110143062 CN 201110143062 A CN201110143062 A CN 201110143062A CN 102275897 A CN102275897 A CN 102275897A
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Abstract
The invention relates to a method for diluting concentrated sulfuric acid by using a mixture of ice and water during a graphite oxide preparation process. The method comprises steps that: graphite powder is placed in a first reaction vessel, concentrated sulfuric acid is then added into the first reaction vessel, and the mixture is stirred; potassium permanganate is added to the first reaction vessel, and the mixture is stirred; the first reaction vessel is heated in a water bath at a temperature of 30 to 40 DEG C; the mixed reactant in the first reaction vessel is added to a second reaction vessel containing a mixture of deionized ice and water, and the mixture is stirred; hydrogen peroxide is gradually dropped into the second reaction vessel until no bubble is generated; insoluble substances in the obtained suspension liquid are obtained by filtering, and are washed several times by using dilute hydrochloric acid and deionized water respectively; the insoluble substances are processed through vacuum filtration, and are dried under room temperature in a vacuum drying oven; after vacuum drying, graphite oxide is obtained. The method provided by the invention has advantages of rapid production, simple and stable technology, low requirement on equipment, and suitability for large-scale productions.
Description
Technical field
The invention belongs to the graphite oxide preparing technical field, especially a kind of method of utilizing the mixture of ice and water dilution vitriol oil in the graphite oxide for preparing.
Background technology
Graphene, English name Graphene is that carbon atom is arranged the two-dimensional crystal lattice structure that forms according to hexagonal.As monolayer carbon atomic plane material, Graphene can obtain by peeling off graphite material.This graphite crystal film is after 2004 are found by the scientist of University of Manchester, and Graphene just becomes the focus that scientific circles and industry member are paid close attention to.The thickness of Graphene has only 0.335 nanometer, is not only in the known materials the thinnest a kind of, also very firmly hard; As simple substance, the speed that it at room temperature transmits electronics than known all conductor and semi-conductor all fast (in the Graphene travelling speed of electronics reached the light velocity 1/300).Because the weird atom structure of Graphene, wherein the behavior of current carrier (electronics and hole) must just can be described with relativistic quantum mechanics (relativistic quantum mechanics).Simultaneously, as the monolayer carbon atomic structure, the theoretical specific surface area of Graphene is up to 2630m
2/ g.So high specific surface area makes becomes extremely promising energy storage active material with the material based on Graphene, makes grapheme material to be applied in storage hydrogen, new type lithium ion battery, ultracapacitor or fuel cell.
At present, its preparation method has multiple, as slight rubbing manipulation or tear tape method (pasting HOPG), heating SiC method, metal substrate chemical Vapor deposition process, chemical dispersion method etc.; Wherein, the most suitable large-scale industrialization of chemical dispersion method is produced grapheme material, and the scope of application is wider.
Prepare the strategic starting point that graphite oxide is considered to extensive synthesizing graphite alkene from graphite, graphite oxide can further be used mechanical means, as ultra-sonic dispersion in pyrolysis expansion or the solvent, the graphene oxide suspension of the accurate two dimension of preparation, increase its mechanical property by surface modification then, and form Graphene through reduction reaction.More difficult hierarchy of control temperature when at present there is the dilution vitriol oil in the graphite oxide preparation method who uses, long reaction time and to problems such as equipment requirements height.Therefore, a kind of fast, technology simple and stable, graphite oxide mass production techniques low for equipment requirements of exploitation just seems particularly important.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, provide a kind of fast, technology simple and stable, low for equipment requirements, a kind of method of utilizing the mixture of ice and water dilution vitriol oil in the graphite oxide for preparing of being suitable for scale operation.
According to technical scheme provided by the invention, a kind of method of utilizing the mixture of ice and water dilution vitriol oil in the graphite oxide for preparing comprises the steps:
A, get Graphite Powder 99 earlier and place first reaction vessel, to add weight percentage again in first reaction vessel be 98% the vitriol oil and stir, and Graphite Powder 99 satisfies with the add-on of the vitriol oil: the vitriol oil of the corresponding 40～50ml of adding of per 1 gram Graphite Powder 99;
B, adding potassium permanganate and stirring in first reaction vessel of step a, the add-on of potassium permanganate satisfies: per 1 gram Graphite Powder 99 correspondence adds 3～4 potassium permanganate that restrain;
C, will place 30～40 ℃ water-bath reacting by heating 1～3 hour at first reaction vessel of step b;
D, the mixed reactant in first reaction vessel after the heating in water bath for reaction joined in second reaction vessel that fills the deionization mixture of ice and water and stir, the amount of deionization mixture of ice and water satisfies in second reaction vessel: the corresponding deionization mixture of ice and water that adds 0.2～0.3L of per 1 gram Graphite Powder 99;
E, continue to stir, hydrogen peroxide is dropwise joined second of steps d answer in the container up to there not being bubble to produce, at this moment, the reactant in second reaction vessel can become glassy yellow suspension;
F, by glass core vacuum apparatus the insolubles in the suspension is filtered out, the insolubles that filters out is washed some times with dilute hydrochloric acid earlier, after dilute hydrochloric acid is washed, respectively washes some times with deionized water;
Insolubles after the washing of g, suction filtration deionization behind the suction filtration placed insolubles under the vacuum drying oven room temperature dry 1～2 day, obtained graphite oxide after the vacuum-drying.
Ice is 1: 1～3: 2 with the mass ratio of water in the described deionization mixture of ice and water of steps d.
In steps d, the mixed reactant in first reaction vessel after the heating in water bath for reaction joined in second reaction vessel that fills the deionization mixture of ice and water and stir and make the hybrid reaction system temperature remain on 0～10 ℃.
Method of the present invention is compared with the existing method that a large amount of deionized waters are slowly joined in the reaction system dilution vitriol oil:
1. can control the temperature of reaction system easily by changing amount that adds mixture of ice and water and the ratio that changes ice and water;
2. can in several minutes, finish the diluting concentrated sulfuric acid process fast;
3. the change of dilution process has reduced its requirement to equipment.Traditional dilution process can cause that when adding water in the vitriol oil system temperature rises, temperature for the hierarchy of control, must utilize a large amount of water of condensation to come system is lowered the temperature in the outside of reactor, this will ask reactor to corrode by anti-strong acid, has simultaneously good heat-conductive characteristic again, just at present, such requirement is difficult to reach; And the dilution process that the present invention proposes only needs the mixed reactant in first reaction vessel joined in second reaction vessel that fills a large amount of deionization mixture of ice and water and gets final product.Therefore have fast, technology simple and stable, low for equipment requirements and be suitable for advantage such as scale operation.
Description of drawings:
Fig. 1 is a process flow sheet of the present invention.
Embodiment
The invention will be further described below in conjunction with specific embodiment.
Embodiment 1
A kind of method of utilizing the mixture of ice and water dilution vitriol oil in the graphite oxide for preparing of the present invention comprises following preparation process:
1, take by weighing 25g hundred rivers 200 order natural flake graphite powder, pour round-bottomed flask into funnel, getting the 1L weight percentage is that 98% vitriol oil is slowly poured round-bottomed flask into, connects electric mixer;
2, setting stirring velocity is 100 rev/mins, takes by weighing 87.5g potassium permanganate, progressively joins in 20 minutes in the vitriol oil Graphite Powder 99 solution;
3, round-bottomed flask is dipped in the water bath, bath temperature is set at 35 ℃ of reactions 2 hours, and mixing speed is made as 200 rev/mins;
4, join (ice: the quality ratio is 1: 1) in the beaker that fills 6L deionization mixture of ice and water after reaction finishes fast, the mixing speed of the electric mixer that is connected in the beaker is 300-400 rev/min, added in 2 minutes, at this moment solution colour becomes brown;
5, continue stirring, is that 30% hydrogen peroxide dropwise joins in the beaker up to there not being bubble to produce with weight percentage, and at this moment solution can become glassy yellow suspension;
6, by glass core vacuum apparatus the insolubles in the glassy yellow suspension being filtered out, is that 10% dilute hydrochloric acid and 1.5L deionized water are respectively washed twice with the 1.5L weight percentage then;
7, suction filtration insolubles up to stripping down from sand core funnel, was put in the vacuum drying oven under the room temperature dry 1-2 days again, obtained the graphite oxide of 51.3g after the vacuum-drying.
Embodiment 2
A kind of method of utilizing the mixture of ice and water dilution vitriol oil in the graphite oxide for preparing of the present invention comprises following preparation process:
1, take by weighing 25g hundred rivers 200 order natural flake graphite powder, pour round-bottomed flask into funnel, getting the 1L weight percentage is that 98% vitriol oil is slowly poured round-bottomed flask into, connects electric mixer;
2, setting stirring velocity is 100 rev/mins, takes by weighing 87.5g potassium permanganate, progressively joins in 20 minutes in the vitriol oil Graphite Powder 99 solution;
3, round-bottomed flask is dipped in the water bath, bath temperature is set at 35 ℃ of reactions 2 hours, and mixing speed is made as 200 rev/mins;
4, join (ice: the quality ratio is 1: 1) in the beaker that fills 5L deionization mixture of ice and water after reaction finishes fast, the mixing speed of the electric mixer that is connected in the beaker is 300-400 rev/min, added in 2 minutes, at this moment solution colour becomes brown;
5, continue stirring, is that 30% hydrogen peroxide dropwise joins in the beaker up to there not being bubble to produce with weight percentage, and at this moment solution can become glassy yellow suspension;
6, by glass core vacuum apparatus the insolubles in the glassy yellow suspension being filtered out, is that 10% dilute hydrochloric acid and 1.5L deionized water are respectively washed twice with the 1.5L weight percentage then;
7, suction filtration insolubles up to stripping down from sand core funnel, was put in the vacuum drying oven under the room temperature dry 1-2 days again, obtained the graphite oxide of 50.8g after the vacuum-drying.
Embodiment 3
A kind of method of utilizing the mixture of ice and water dilution vitriol oil in the graphite oxide for preparing of the present invention comprises following preparation process:
1, take by weighing 25g hundred rivers 200 order natural flake graphite powder, pour round-bottomed flask into funnel, getting the 1.25L weight percentage is that 98% vitriol oil is slowly poured round-bottomed flask into, connects electric mixer;
2, setting stirring velocity is 100 rev/mins, takes by weighing 87.5g potassium permanganate, progressively joins in 20 minutes in the vitriol oil Graphite Powder 99 solution;
3, round-bottomed flask is dipped in the water bath, bath temperature is set at 35 ℃ of reactions 1 hour, and mixing speed is made as 200 rev/mins;
4, join (ice: the quality ratio is 3: 2) in the beaker that fills 6.25L deionization mixture of ice and water after reaction finishes fast, the mixing speed of the electric mixer that is connected in the beaker is 300-400 rev/min, added in 2 minutes, at this moment solution colour becomes brown;
5, continue stirring, is that 30% hydrogen peroxide dropwise joins in the beaker up to there not being bubble to produce with weight percentage, and at this moment solution can become glassy yellow suspension;
6, by glass core vacuum apparatus the insolubles in the glassy yellow suspension being filtered out, is that 10% dilute hydrochloric acid and 1.5L deionized water are respectively washed twice with the 1.5L weight percentage then;
7, suction filtration insolubles up to stripping down from sand core funnel, was put in the vacuum drying oven under the room temperature dry 1-2 days again, obtained the graphite oxide of 49.3g after the vacuum-drying.
Embodiment 4
A kind of method of utilizing the mixture of ice and water dilution vitriol oil in the graphite oxide for preparing of the present invention comprises following preparation process:
1, take by weighing 25g hundred rivers 200 order natural flake graphite powder, pour round-bottomed flask into funnel, getting the 1L weight percentage is that 98% vitriol oil is slowly poured round-bottomed flask into, connects electric mixer;
2, setting stirring velocity is 100 rev/mins, takes by weighing 75g potassium permanganate, progressively joins in 20 minutes in the vitriol oil Graphite Powder 99 solution;
3, round-bottomed flask is dipped in the water bath, bath temperature is set at 35 ℃ of reactions 2 hours, and mixing speed is made as 200 rev/mins;
4, join (ice: the quality ratio is 3: 2) in the beaker that fills 5L deionization mixture of ice and water after reaction finishes fast, add in 5 minutes under need not condition of stirring, at this moment solution colour becomes brown;
5, be that 30% hydrogen peroxide dropwise joins in the beaker up to there not being bubble to produce with weight percentage, at this moment solution can become glassy yellow suspension;
6, by glass core vacuum apparatus the insolubles in the glassy yellow suspension being filtered out, is that 10% dilute hydrochloric acid and 1.5L deionized water are respectively washed twice with the 1.5L weight percentage then;
7, suction filtration insolubles up to stripping down from sand core funnel, was put in the vacuum drying oven under the room temperature dry 1-2 days again, obtained the graphite oxide of 50.7g after the vacuum-drying.
Embodiment 5
A kind of method of utilizing the mixture of ice and water dilution vitriol oil in the graphite oxide for preparing of the present invention comprises following preparation process:
1, take by weighing 20g hundred rivers 200 order natural flake graphite powder, pour round-bottomed flask into funnel, getting the 0.90L weight percentage is that 98% vitriol oil is slowly poured round-bottomed flask into, connects electric mixer;
2, setting stirring velocity is 100 rev/mins, takes by weighing 80g potassium permanganate, progressively joins in 20 minutes in the vitriol oil Graphite Powder 99 solution;
3, round-bottomed flask is dipped in the water bath, bath temperature is set at 35 ℃ of reactions 3 hours, and mixing speed is made as 200 rev/mins;
4, join (ice: the quality ratio is 1.25: 1) in the beaker that fills 6L deionization mixture of ice and water after reaction finishes fast, add in 5 minutes under need not condition of stirring, at this moment solution colour becomes brown;
5, be that 30% hydrogen peroxide dropwise joins in the beaker up to there not being bubble to produce with weight percentage, at this moment solution can become glassy yellow suspension;
6, by glass core vacuum apparatus the insolubles in the glassy yellow suspension being filtered out, is that 10% dilute hydrochloric acid and 1.5L deionized water are respectively washed twice with the 1.5L weight percentage then;
7, suction filtration insolubles up to stripping down from sand core funnel, was put in the vacuum drying oven under the room temperature dry 1～2 day again, obtained the graphite oxide of about 51.2g after the vacuum-drying.
As can be seen from the above embodiments, the graphite oxide weight that obtains is about the twice of Graphite Powder 99 raw material weight, has illustrated that the slotting oxygen degree of graphite oxide of the inventive method preparation is higher.
Claims (3)
1. one kind prepares the method for utilizing the mixture of ice and water dilution vitriol oil in the graphite oxide, it is characterized in that this method comprises the steps:
A, get Graphite Powder 99 earlier and place first reaction vessel, to add weight percentage again in first reaction vessel be 98% the vitriol oil and stir, and Graphite Powder 99 satisfies with the add-on of the vitriol oil: the vitriol oil of the corresponding 40～50ml of adding of per 1 gram Graphite Powder 99;
B, adding potassium permanganate and stirring in first reaction vessel of step a, the add-on of potassium permanganate satisfies: per 1 gram Graphite Powder 99 correspondence adds 3～4 potassium permanganate that restrain;
C, first reaction vessel of step b placed 30～40 ℃ water-bath reacting by heating 1～3 hour;
D, the mixed reactant in first reaction vessel after the heating in water bath for reaction joined in second reaction vessel that fills the deionization mixture of ice and water and stir, the add-on of deionization mixture of ice and water satisfies in second reaction vessel: the corresponding deionization mixture of ice and water that adds 0.2～0.3L of per 1 gram Graphite Powder 99;
E, continue to stir, hydrogen peroxide is dropwise joined second of steps d answer in the container up to there not being bubble to produce, at this moment, the reactant in second reaction vessel can become glassy yellow suspension;
F, the insolubles in the suspension is filtered out by glass core vacuum apparatus, the insolubles that filters out earlier with dilute hydrochloric acid wash some all over after, wash some times with deionized water;
Insolubles after the washing of g, suction filtration deionization behind the suction filtration placed insolubles under the vacuum drying oven room temperature dry 1～2 day, obtained graphite oxide after the vacuum-drying.
2. a kind of method of utilizing the mixture of ice and water dilution vitriol oil in the graphite oxide for preparing as claimed in claim 1, it is characterized in that: ice is 1: 1～3: 2 with the mass ratio of water in the described deionization mixture of ice and water of steps d.
3. a kind of method of utilizing the mixture of ice and water dilution vitriol oil in the graphite oxide for preparing as claimed in claim 1, it is characterized in that: in steps d, the mixed reactant in first reaction vessel after the heating in water bath for reaction joined in second reaction vessel that fills the deionization mixture of ice and water and stir and make the hybrid reaction system temperature remain on 0～10 ℃.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105347335A (en) * | 2015-11-27 | 2016-02-24 | 湖北大学 | Method for preparing graphene oxide by taking K2FeO4 as oxidizing agent |
| WO2017147468A1 (en) * | 2016-02-26 | 2017-08-31 | Nanotech Energy, Inc. | Methods, devices and systems for processing of carbonaceous compositions |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2798878A (en) * | 1954-07-19 | 1957-07-09 | Nat Lead Co | Preparation of graphitic acid |
| CN101941694A (en) * | 2010-09-07 | 2011-01-12 | 湘潭大学 | Preparation method of high-dispersivity graphene |
-
2011
- 2011-05-30 CN CN 201110143062 patent/CN102275897A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2798878A (en) * | 1954-07-19 | 1957-07-09 | Nat Lead Co | Preparation of graphitic acid |
| CN101941694A (en) * | 2010-09-07 | 2011-01-12 | 湘潭大学 | Preparation method of high-dispersivity graphene |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105347335A (en) * | 2015-11-27 | 2016-02-24 | 湖北大学 | Method for preparing graphene oxide by taking K2FeO4 as oxidizing agent |
| WO2017147468A1 (en) * | 2016-02-26 | 2017-08-31 | Nanotech Energy, Inc. | Methods, devices and systems for processing of carbonaceous compositions |
| US9782739B2 (en) | 2016-02-26 | 2017-10-10 | Nanotech Energy, Inc. | Methods, devices and systems for processing of carbonaceous compositions |
| US10112167B2 (en) | 2016-02-26 | 2018-10-30 | Nanotech Energy, Inc. | Methods, devices and systems for processing of carbonaceous compositions |
| CN109071234A (en) * | 2016-02-26 | 2018-12-21 | 纳米技术能源公司 | For handling the methods, devices and systems of carbonaceous composition |
| JP2019507717A (en) * | 2016-02-26 | 2019-03-22 | ナノテック エナジー，インク． | Method, apparatus, and system for treating carbonaceous compositions |
| US10449505B2 (en) | 2016-02-26 | 2019-10-22 | Nanotech Energy, Inc. | Methods, devices and systems for processing of carbonaceous compositions |
| US11192082B2 (en) | 2016-02-26 | 2021-12-07 | Nanotech Energy, Inc. | Methods, devices and systems for processing of carbonaceous compositions |
| US11752479B2 (en) | 2016-02-26 | 2023-09-12 | Nanotech Energy, Inc. | Methods, devices and systems for processing of carbonaceous compositions |
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