CN105502357A - Stripping agent special for preparing graphene through mechanical stripping and preparation method - Google Patents
Stripping agent special for preparing graphene through mechanical stripping and preparation method Download PDFInfo
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- CN105502357A CN105502357A CN201510965632.6A CN201510965632A CN105502357A CN 105502357 A CN105502357 A CN 105502357A CN 201510965632 A CN201510965632 A CN 201510965632A CN 105502357 A CN105502357 A CN 105502357A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/04—Specific amount of layers or specific thickness
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
Abstract
The invention discloses a stripping agent special for preparing graphene through mechanical stripping and a preparation method. The stripping agent is prepared from, by weight, 25%-35% of composite nanoparticles, 1%-5% of dispersing agent and 60%-74% of deionized water, wherein the preparation method comprises the steps that metal or metallic oxide nano powder is taken as the main body which is wrapped with graphene oxide, amino groups are grafted onto the graphene oxide, and then the composite nanoparticles are formed. By means of the method, the stripping agent special for preparing the graphene through mechanical stripping is provided, the space between graphitic layers can be effectively widened, graphite can be stripped in a pollution-free mode, and agglomeration of the graphene can be prevented.
Description
Technical field
The present invention relates to technical field of nanometer material preparation, particularly special stripper of a kind of mechanically peel Graphene and preparation method thereof.
Background technology
Graphene is the Two-dimensional Carbon atomic crystal in recent years found, is one of the study hotspot in current carbonaceous material and Condensed Matter Physics field.Graphene constructs the sp such as zero dimension soccerballene, one dimension carbon nanotube, said three-dimensional body phase graphite
2the basic structural unit of hydridization carbon.Although Graphene only has a carbon atom thickness, be also that oneself knows one the thinnest in material, but Graphene very rigid.In addition, carbon atom has four valence electrons, and each like this carbon atom can contribute the π-electron of a non-Cheng Jian, and these π-electrons become vertical direction can form π track with plane, π-electron then can move freely in crystal, gives the electroconductibility that Graphene is good.The characteristic of these excellences makes Graphene have very vast potential for future development.
In order to allow outstanding grapheme material realize suitability for industrialized production and application, a kind of can be mass-produced and the number of plies and the controlled preparation method of size just must be developed.The preparation method of current Graphene has mechanical stripping method, epitaxial growth method, oxidation reduction process, ultrasonic stripping method, organic synthesis method, solvent-thermal method, chemical Vapor deposition process etc.In these methods, because mechanically peel method can preserve the character of Graphene best, and preparation method is simple, and preparation process is environment friendly and pollution-free, in the production of reality, enjoy favor.
China Patent Publication No. 102874797A discloses a kind of method preparing high-quality graphene on a large scale, and expanded graphite is scattered in stripper solution and stirs dipping by the method, after filtration, and washing, dry obtained Graphene.The present invention has preparation condition gentleness, simple to operate, easily accomplish scale production advantage.But the method is owing to adopting the graphite after ultrasonic immersing stripper, and to the finite energy of graphite and stripper compound system, therefore, the probability opening graphite layers Van der Waals force is very low, thus the productive rate of Graphene is very low.
The preparation method that China Patent Publication No. 102701187A discloses a kind of Graphene and the Graphene using the method to prepare.This invention take graphite as raw material, obtaining compound between graphite layers, then peeling off described compound between graphite layers and obtaining Graphene by inserting metal in graphite layers.The method utilizes metal as stripper, and preparation method is easy, with low cost.But, the method is after in stripping process, metal enters graphite layers, metal is at graphite layers accumulative crystallization, or formed in the process of carbide, atoms metal is direction-free grows up, and causes graphene sheet layer to be penetrated, and reduces the size of Graphene, destroy the two-dimensional physical structure of graphite flake layer, its mechanical property and conductivity are deteriorated.
China Patent Publication No. 103935999A discloses a kind of preparation method of Graphene.The method take polar solvent as dispersion medium, high-quality graphene is prepared by mechanically peel method under graphene quantum dot is auxiliary, mainly utilize the dispersiveness that graphene quantum dot is good in polar solvent, and stronger non covalent bond is combined between Graphene/graphene sheet layer, promote stripping and the dispersion of graphene nanometer sheet in polar solvent of natural graphite, thus obtain high-quality Graphene.The method is simple to operate, but the Graphene obtained is combined closely with stripper or dispersion agent, is difficult to purifying and transfer.
In sum, namely present existing mechanically peel legal system can expand graphite layers distance effectively for also not having one in the technology of Graphene, and contamination-freely peel off graphite, the mechanically peel that Graphene can also be stoped to reunite prepares the special stripper of Graphene.
Summary of the invention
In order to solve deficiency and the defect of aforesaid method, the present invention develops a kind of mechanically peel and prepares the special stripper of Graphene.The method adopts the main body of nanoparticle as stripper of the graphene oxide parcel of grafted amino group acid, the π key utilizing graphene oxide to have and Graphene form π-π and act on, utilize the sharpened surface of nanoparticle, insert graphite layers and peel off Graphene, utilize the protonated Graphene that makes of the amino group of graft product charged, rely on Coulomb repulsion to stop the reunion of Graphene.
On the one hand, the invention provides a kind of mechanically peel and prepare the special stripper of Graphene, it is characterized in that, described stripper consists of the following composition, and comprising: the composite nano particle of weight percent 25 ~ 35%, the dispersion agent of 1 ~ 5% and the deionized water of 60 ~ 74%;
Wherein, described composite nano particle is main body by metal or metal oxide nano powder, is surrounded by graphene oxide, the Structure composing of grafted amino group group on graphene oxide.
Preferably, described metal or metal oxide nano powder diameter of particle are 20 ~ 50nm, and the sheet footpath of described graphene oxide is 100-300nm.
Preferably, described metal or metal oxide nanoparticles and graphene oxide mass ratio are 2 ~ 8:1.
Preferably, described metal or metal oxide nano powder are nanometer iron powder, copper nanoparticle, Nano-sized Ferric Oxide Powder, nano oxidized copper powder, one or more in nano alumina powder; Described amino group derives from one or more in leucine, Isoleucine, methionine(Met), aspartic acid, L-glutamic acid, Methionin, arginine, glycine, Serine, Threonine, L-Ala, phenylalanine.
Preferably, described dispersion agent is one or more in sodium lauryl sulphate, sodium laurylsulfonate and polyvinylpyrrolidone.
On the other hand, the invention provides the preparation method that a kind of mechanically peel prepares the special stripper of Graphene, it is characterized in that, comprise the following steps:
By metal or metal oxide nanoparticles and graphene oxide blended, add deionized water and dispersion agent, stir with stirrer, be heated to 50 ~ 80 DEG C, obtain turbid solution;
Amino acid is added in previous step turbid solution, keep stirring 3 ~ 5 hours, utilize esterification by amino group graft in described surface of graphene oxide, reduce temperature to room temperature, obtain stripper.
Preferably, described stirrer stirring velocity is 40 ~ 80 revs/min.
Above-mentioned one or more technical scheme in the embodiment of the present application, at least has one or more technique effects following:
1, this kind of stripper is in stripping Graphene process, has provide protection, avoid the increase of Graphene self-defect to Graphene.And, to a certain extent, to the Graphene peeled off, there is repair.
2, in this kind of stripper, the protonated Graphene that makes of the amino group of graft product is charged, relies on Coulomb repulsion to stop the reunion of Graphene, is convenient to obtain the smooth Graphene of high-quality.
3, this kind of stripper, owing to containing metal or metal oxide microparticle in nanoparticle, relative density increases, and is convenient to the centrifugation in later stage, reduces the impurity in graphene product.
Embodiment
By embodiment, the present invention is described in further detail, but this should be interpreted as scope of the present invention is only limitted to following example.When not departing from aforesaid method thought of the present invention, the various replacement made according to ordinary skill knowledge and customary means or change, all should be within the scope of the present invention.
Embodiment one
In the present embodiment, the composition of stripper is as follows:
Composite nano particle, weight percent is 25%; Sodium lauryl sulphate, weight percent is 2%; And deionized water, weight percent is 73%.
Stripper is prepared from by step below:
The graphene oxide that to choose particle diameter be metallic iron nanoparticle and the sheet footpath of 20nm is 100nm mixes, metallic iron nanoparticle and graphene oxide mass ratio are 2:1, add appropriate dispersion agent sodium lauryl sulphate and appropriate amount of deionized water, stir with stirrer, the stirring velocity arranging stirrer is 40 revs/min, be heated to 50 DEG C, obtain turbid solution.The leucine that graphene oxide 1/3 measures is added in above-mentioned turbid solution, leave standstill 12h, after reaction to be esterified terminates, reduce temperature to room temperature, and then acquisition contains based on metallic iron nanometer powder, wrap up graphene oxide outside metallic iron nano-powder, on graphene oxide, the solvent of the composite nano particle of grafted amino group group is that mechanically peel prepares the special stripper of Graphene.
Stripper and the expanded graphite mass ratio of preparation in Example one are 1:50, and the Graphene prepared is of a size of 2.09 μm (selected area sizes), and thickness is 0.83nm, and productive rate is 11.5%.
Embodiment two
Composite nano particle, weight percent is 25%; Sodium lauryl sulphate, weight percent is 2%; And deionized water, weight percent is 73%.
Stripper is prepared from by step below:
The graphene oxide that to choose particle diameter be metallic iron nanoparticle and the sheet footpath of 40nm is 300nm mixes, metallic iron nanoparticle and graphene oxide mass ratio are 4:1, add appropriate dispersion agent sodium lauryl sulphate and appropriate amount of deionized water, stir with stirrer, the stirring velocity arranging stirrer is 40 revs/min, be heated to 50 DEG C, obtain turbid solution.The leucine that graphene oxide 1/3 measures is added in above-mentioned turbid solution, leave standstill 12h, after reaction to be esterified terminates, reduce temperature to room temperature, and then acquisition contains based on metallic iron nanometer powder, wrap up graphene oxide outside metallic iron nano-powder, on graphene oxide, the solvent of the composite nano particle of grafted amino group group is that mechanically peel prepares the special stripper of Graphene.
Stripper and the expanded graphite mass ratio of preparation in Example two are 1:50, and the Graphene prepared is of a size of 3.23 μm (selected area sizes), and thickness is 0.82nm, and productive rate is 10.7%.
Embodiment three
Composite nano particle, weight percent is 35%; Sodium laurylsulfonate, weight percent is 1%; And deionized water, weight percent is 64%.
Stripper is prepared from by step below:
The graphene oxide that to choose particle diameter be metallic iron nanoparticle and the sheet footpath of 40nm is 300nm mixes, metallic iron nanoparticle and graphene oxide mass ratio are 4:1, add appropriate dispersion agent sodium lauryl sulphate and appropriate amount of deionized water, stir with stirrer, the stirring velocity arranging stirrer is 40 revs/min, be heated to 50 DEG C, obtain turbid solution.The leucine that graphene oxide 1/3 measures is added in above-mentioned turbid solution, leave standstill 12h, after reaction to be esterified terminates, reduce temperature to room temperature, and then acquisition contains based on metallic iron nanometer powder, wrap up graphene oxide outside metallic iron nano-powder, on graphene oxide, the solvent of the composite nano particle of grafted amino group group is that mechanically peel prepares the special stripper of Graphene.
Stripper and the expanded graphite mass ratio of preparation in Example three are 1:50, and the Graphene prepared is of a size of 2.09 μm (selected area sizes), and thickness is 0.83nm, and productive rate is 17.5%.
Embodiment four
Composite nano particle, weight percent is 35%; Sodium laurylsulfonate, weight percent is 1%; And deionized water, weight percent is 64%.
Stripper is prepared from by step below:
The graphene oxide that to choose particle diameter be nano alumina particles and the sheet footpath of 40nm is 300nm mixes, nano alumina particles and graphene oxide mass ratio are 4:1, add appropriate dispersion agent sodium lauryl sulphate and appropriate amount of deionized water, stir with stirrer, the stirring velocity arranging stirrer is 40 revs/min, be heated to 50 DEG C, obtain turbid solution.The L-Ala that graphene oxide 1/3 measures is added in above-mentioned turbid solution, leave standstill 12h, after reaction to be esterified terminates, reduce temperature to room temperature, and then acquisition contains based on metallic iron nanometer powder, wrap up graphene oxide outside nano aluminium oxide, on graphene oxide, the solvent of the composite nano particle of grafted amino group group is that mechanically peel prepares the special stripper of Graphene.
Stripper and the expanded graphite mass ratio of preparation in Example four are 1:50, and the Graphene prepared is of a size of 4.01 μm (selected area sizes), and thickness is 0.97nm, and productive rate is 17.2%.
Embodiment five
Composite nano particle, weight percent is 35%; Sodium laurylsulfonate, weight percent is 1%; And deionized water, weight percent is 64%.
Stripper is prepared from by step below:
The graphene oxide that to choose particle diameter be nano alumina particles and the sheet footpath of 50nm is 300nm mixes, nano alumina particles and graphene oxide mass ratio are 8:1, add appropriate dispersion agent sodium lauryl sulphate and appropriate amount of deionized water, stir with stirrer, the stirring velocity arranging stirrer is 80 revs/min, be heated to 80 DEG C, obtain turbid solution.The Serine that graphene oxide 1/4 mole measures is added in above-mentioned turbid solution, leave standstill 12h, after reaction to be esterified terminates, reduce temperature to room temperature, and then acquisition contains based on metallic iron nanometer powder, wrap up graphene oxide outside nano aluminium oxide, on graphene oxide, the solvent of the composite nano particle of grafted amino group group is that mechanically peel prepares the special stripper of Graphene.
Stripper and the expanded graphite mass ratio of preparation in Example five are 1:50, and the Graphene prepared is of a size of 1.59 μm (selected area sizes), and thickness is 0.77nm, and productive rate is 15.3%
Although describe the preferred embodiments of the present invention, those skilled in the art once obtain the basic creative concept of cicada, then can make other change and amendment to these embodiments.So claims are intended to be interpreted as comprising preferred embodiment and falling into all changes and the amendment of the scope of the invention.
Obviously, those skilled in the art can carry out various change and modification to the present invention and not depart from the spirit and scope of the present invention.Like this, if these amendments of the present invention and modification belong within the scope of the claims in the present invention and equivalent technologies thereof, then the present invention is also intended to comprise these change and modification.
Claims (7)
1. mechanically peel prepares the special stripper of Graphene, it is characterized in that, described stripper consists of the following composition, and comprising: the composite nano particle of weight percent 25 ~ 35%, the dispersion agent of 1 ~ 5% and the deionized water of 60 ~ 74%;
Wherein, described composite nano particle is main body by metal or metal oxide nano powder, is surrounded by graphene oxide, the Structure composing of grafted amino group group on graphene oxide.
2. a kind of mechanically peel according to claim 1 prepares the special stripper of Graphene, it is characterized in that, described metal or metal oxide nano powder diameter of particle are 20 ~ 50nm, and the sheet footpath of described graphene oxide is 100-300nm.
3. a kind of mechanically peel according to claim 1 prepares the special stripper of Graphene, it is characterized in that, described metal or metal oxide nanoparticles and graphene oxide mass ratio are 2 ~ 8:1.
4. a kind of mechanically peel according to claim 1 prepares the special stripper of Graphene, it is characterized in that, described metal or metal oxide nano powder are nanometer iron powder, copper nanoparticle, Nano-sized Ferric Oxide Powder, nano oxidized copper powder, one or more in nano alumina powder; Described amino group derives from one or more in leucine, Isoleucine, methionine(Met), aspartic acid, L-glutamic acid, Methionin, arginine, glycine, Serine, Threonine, L-Ala, phenylalanine.
5. a kind of mechanically peel according to claim 1 prepares the special stripper of Graphene, it is characterized in that, described dispersion agent is one or more in sodium lauryl sulphate, sodium laurylsulfonate and polyvinylpyrrolidone.
6. a kind of mechanically peel according to claim 1 prepares a preparation method for the special stripper of Graphene, it is characterized in that, comprises the following steps:
A. by metal or metal oxide nanoparticles and graphene oxide blended, add deionized water and dispersion agent, stir with stirrer, be heated to 50 ~ 80 DEG C, obtain turbid solution;
B. amino acid is added in the turbid solution of a step, keep stirring 3 ~ 5 hours, utilize esterification by amino group graft in described surface of graphene oxide, reduce temperature to room temperature, obtain stripper.
7. a kind of mechanically peel according to claim 6 prepares the preparation method of the special stripper of Graphene, it is characterized in that, described stirrer stirring velocity is 40 ~ 80 revs/min.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106517166A (en) * | 2016-10-19 | 2017-03-22 | 成都新柯力化工科技有限公司 | Composite stripping agent used for preparing graphene in stripping manner through slurry stirring |
| CN106744870A (en) * | 2016-10-25 | 2017-05-31 | 成都新柯力化工科技有限公司 | A kind of abrasive media that Graphene is peeled off for slurry grinding |
| CN107857260A (en) * | 2017-12-13 | 2018-03-30 | 西北有色金属研究院 | A kind of method that weak oxide intercalation stripping prepares graphene oxide |
| CN107936159A (en) * | 2017-12-22 | 2018-04-20 | 安徽工业大学 | A kind of preparation method of the high quick selfreparing physical hydrogel of stretching |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106517166A (en) * | 2016-10-19 | 2017-03-22 | 成都新柯力化工科技有限公司 | Composite stripping agent used for preparing graphene in stripping manner through slurry stirring |
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| CN107857260A (en) * | 2017-12-13 | 2018-03-30 | 西北有色金属研究院 | A kind of method that weak oxide intercalation stripping prepares graphene oxide |
| CN107936159A (en) * | 2017-12-22 | 2018-04-20 | 安徽工业大学 | A kind of preparation method of the high quick selfreparing physical hydrogel of stretching |
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| CN105502357B (en) | 2017-05-31 |
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