CN104860301A - Composite inflation liquid - Google Patents
Composite inflation liquid Download PDFInfo
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- CN104860301A CN104860301A CN201510186549.9A CN201510186549A CN104860301A CN 104860301 A CN104860301 A CN 104860301A CN 201510186549 A CN201510186549 A CN 201510186549A CN 104860301 A CN104860301 A CN 104860301A
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- expanded liquid
- composite expanded
- metal ion
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- superoxol
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Abstract
The invention discloses a composite inflation liquid which is characterized in that the inflation liquid is prepared by uniformly mixing the following components, by mass: 60-90% of a hydrogen peroxide solution, 1-10% of a metal ion complexing agent, 1-5% of a pH value adjusting agent, 0.5-5% of a surface tension adjusting agent, and balance of water. With the inflation liquid, metal ions in a solution can be absorbed during an inflation reaction, such that the metal ions lose their catalytic activity. Effective decomposition is promoted, and ineffective decomposition is inhibited, such that a graphite intercalation compound can be inflated completely and thoroughly.
Description
Technical field
The present invention relates to field of graphene, relate in particular to a kind of composite expanded liquid, this composite expanded liquid is mainly used in expansion process graphite intercalation compound, is especially applicable to mass-producing process graphite intercalation compound.
Background technology
Since being found from 2004, Graphene receives much concern as a kind of new carbon.It is a kind of completely by
sp 2 the thickness of the carbon atom formation of hydridization is only the accurate two dimensional crystal material of monoatomic layer or several monoatomic layer, there is the performance that high light transmittance and electroconductibility, high-specific surface area, high strength and snappiness etc. are excellent, be expected to obtain widespread use in fields such as high-performance nanometer electronic device, photoelectric device, gas sensor, matrix material, field emmision material and stored energies.
At present, the grapheme material that academia accepts extensively is defined as: the graphite flake of the carbon atom number of plies within 10 layers, its thickness is below 3.5 nanometers.For this reason, China Patent No. " 201110282370.5 " disclosed " a kind of method preparing high-quality graphene " on May 2nd, 2012, its technical scheme is for raw material with halogen or the metal halide graphite intercalation compound that is intercalator, expansion and ultrasonic stripping is in a solvent carried out in oxalic acid or superoxol, thus obtain high-quality graphene, the method can realize the preparation of the high-quality graphene of single batch of hectogram level, the characteristic property index of gained graphene product is: the number of plies 3-8 layers (thickness is 1-2.5 nanometers) of graphene film, lateral dimension 5-50 microns, carbon-to-oxygen ratio 30-120, foreign matter content 5 wt%.
The preparation principle of aforesaid method is: as shown in Figure 1, under the condition that liquid phase is soaked, utilizes the metal ion (M being present in graphite layers
x+) catalyzing hydrogen peroxide decomposes at interlayer and to produce oxygen (O
2) expansion peel off graphite obtain Graphene, its core reaction is:
Wherein, the cartalytic decomposition effect occurring in graphite layers becomes effective decomposition, graphite expansion can be made to prepare Graphene, the cartalytic decomposition effect occurred in particles of intercalated graphite external solution is then decomposition, the consumption of reactant can be caused, reactant can be stoped simultaneously to the diffusion of graphite layers, thus suppress effectively to decompose, cause the deterioration of intercalated graphite expansion effect; Therefore, the key preparing Graphene suppresses decomposition while being to promote effectively to decompose.At first, metal ion is only present in graphite layers, therefore reacts effectively to be decomposed into master; But along with the carrying out of reaction and the stripping of graphite flake layer, interlayer metal ion is dissolved in liquid phase gradually, when the concentration of metal ion increases to a certain degree, can cause the aggravation of decomposition.Particularly when a large amount of preparation the Graphene of hundreds of kilograms (single batch preparation), the increase of inventory, cause from the amount of metal ion of graphite layers stripping huge, otherwise increasing of material also makes metal ion diffusion hindered in the solution, but because the inflation fluid in above-mentioned patent is oxalic acid or superoxol, this inflation fluid can not be processed the metal ion in solution, this just causes local invalid to decompose aggravation, make the working substance Mass lost participating in expansion reaction, cause the underexpansion of intercalated graphite raw material, and then the expansion of graphite is had a negative impact.
Summary of the invention
The object of the invention is to solve the above-mentioned problems in the prior art, a kind of composite expanded liquid is provided, the present invention can metal ion in expansion reaction process in adsorbent solution, metal ion is made to lose catalytic activity, while promotion is effectively decomposed, suppress decomposition, ensure that graphite intercalation compound can fully and completely expand.
For achieving the above object, the technical solution used in the present invention is as follows:
A kind of composite expanded liquid, it is characterized in that being formed by following component Homogeneous phase mixing, the mass percent of each component and each component is: superoxol 60-90%, complexing of metal ion agent 1-10%, acidity-basicity regulator 1-5%, surface tension modifier 0.5-5%, all the other are water.
In described composite expanded liquid, the mass percent of superoxol is 85%, and the mass percent of complexing of metal ion agent is 5%, and the mass percent of acidity-basicity regulator is 3%, and the mass percent of surface tension modifier is 2%, and all the other are water.
The concentration of described superoxol is 20-30%.
Complexing of metal ion agent in described composite expanded liquid is one or more the compound in Seignette salt, trisodium phosphate, disodium edta, oxalic acid, oxalate, Sunmorl N 60S, ethylenediamine tetraacetic methene sodium phosphate, diethanolamine, trolamine.
Acidity-basicity regulator in described composite expanded liquid is one or more the compound in hydrochloric acid, sulfuric acid, phosphoric acid, oxalic acid, formic acid, acetic acid, oxalic acid, ammoniacal liquor, sodium hydroxide, potassium hydroxide, quadrol, sodium bicarbonate.
Surface tension modifier in described composite expanded liquid is one or more the compound in methyl alcohol, ethanol, propyl alcohol, butanols, ethyl acetate, Sodium dodecylbenzene sulfonate.
Employing the invention has the advantages that:
One, the composite expanded liquid in the present invention is formed by superoxol, complexing of metal ion agent, acidity-basicity regulator, surface tension modifier and water Homogeneous phase mixing, and wherein, the effect of superoxol is and the metal ion (M being present in graphite layers
x+) react, decompose the oxygen (O produced
2) expansion is risen to graphite intercalation compound; The effect of complexing of metal ion agent is then adsorb the metal ion be dissolved in solution, makes it lose catalytic activity, reaches the effect suppressing decomposition; The effect of acidity-basicity regulator is adjustment inflation fluid and potential of hydrogen, optimizes the complexing effect of metal ionic complexing agent; The effect of surface tension modifier is adjustment stripping liquid to the wetting property of graphite and Graphene, to promote that swelling agent is to the diffusion of graphite layers, and then promotes effective decomposition reaction.The composite expanded liquid be made up of above-mentioned specific component and content, can metal ion in expansion reaction process in adsorbent solution, make metal ion lose catalytic activity, while promotion is effectively decomposed, suppress decomposition, ensure that graphite intercalation compound can fully and completely expand.Compared with the prior art be " 201110282370.5 " with China Patent No. being representative, the present invention is not only specially adapted to mass-producing and prepares graphene product, and the manufacture of also producing hundreds of kilograms of Graphenes for single batch provides powerful guarantee.
Two, in the present invention, if the concentration of superoxol is lower than 20%, the reaction times will be caused long insufficient with reaction; If the concentration of superoxol is higher than 30%, there is again reaction aggravation, react the safety problem such as uncontrollable, therefore the concentration of superoxol is set as 20-30%, has both ensure that mildness and the security of reaction, in turn ensure that the adequacy of reaction.
Three, in the present invention, complexing of metal ion agent, acidity-basicity regulator and surface tension modifier all can be made up of one or more materials, have raw material and are easy to get and advantage with low cost.
Accompanying drawing explanation
Fig. 1 is the expansion release mechanism schematic diagram that graphite intercalation compound uses composite expanded liquid: (a) graphite intercalation compound joins in superoxol; B () hydrogen peroxide decomposes generation oxygen (O2) under the katalysis of graphite layers metal ion; Occur under c effect that () graphene sheet layer expands at oxygen to peel off the Graphene obtaining monolithic.
Embodiment
Embodiment 1
A kind of composite expanded liquid, formed by following component Homogeneous phase mixing, the mass percent of each component and each component is: superoxol 90%, complexing of metal ion agent 1%, acidity-basicity regulator 5%, surface tension modifier 0.5%, and all the other are water.Wherein, the concentration of described superoxol is 20%, complexing of metal ion agent in described composite expanded liquid is one or both the compound in Seignette salt and trisodium phosphate, acidity-basicity regulator in described composite expanded liquid is one or both the compound in hydrochloric acid and sulfuric acid, and the surface tension modifier in described composite expanded liquid is one or both the compound in methyl alcohol and ethanol.
In the present embodiment, the experiment proved that, for the graphite intercalation compound of 4 parts of identical amounts, use respectively through the composite expanded liquid expansion process 40min obtained by above-mentioned special parameter, 60min, 100min and 120min, following experimental result can be obtained:
Embodiment 2
A kind of composite expanded liquid, formed by following component Homogeneous phase mixing, the mass percent of each component and each component is: superoxol 85%, complexing of metal ion agent 5%, acidity-basicity regulator 3%, surface tension modifier 2%, and all the other are water.Wherein, the concentration of described superoxol is 24%, complexing of metal ion agent in described composite expanded liquid is one or more the compound in trisodium phosphate, disodium edta and oxalic acid, acidity-basicity regulator in described composite expanded liquid is one or more the compound in phosphoric acid, oxalic acid, formic acid and acetic acid, and the surface tension modifier in described composite expanded liquid is one or both the compound in propyl alcohol and butanols.
In the present embodiment, the experiment proved that, for the graphite intercalation compound of 4 parts of identical amounts, use respectively through the composite expanded liquid expansion process 40min obtained by above-mentioned special parameter, 60min, 100min and 120min, following experimental result can be obtained:
Embodiment 3
A kind of composite expanded liquid, formed by following component Homogeneous phase mixing, the mass percent of each component and each component is: superoxol 80%, complexing of metal ion agent 8%, acidity-basicity regulator 5%, surface tension modifier 3.5%, and all the other are water.Wherein, the concentration of described superoxol is 27%, complexing of metal ion agent in described composite expanded liquid is one or both compounds in oxalate and Sunmorl N 60S, acidity-basicity regulator in described composite expanded liquid is one or more the compound in oxalic acid, ammoniacal liquor, sodium hydroxide and potassium hydroxide, and the surface tension modifier in described composite expanded liquid is one or both the compound in butanols and ethyl acetate.
In the present embodiment, the experiment proved that, for the graphite intercalation compound of 4 parts of identical amounts, use respectively through the composite expanded liquid expansion process 40min obtained by above-mentioned special parameter, 60min, 100min and 120min, following experimental result can be obtained:
Embodiment 4
A kind of composite expanded liquid, formed by following component Homogeneous phase mixing, the mass percent of each component and each component is: superoxol 75%, complexing of metal ion agent 10%, acidity-basicity regulator 4%, surface tension modifier 5%, and all the other are water.Wherein, the concentration of described superoxol is 30%, complexing of metal ion agent in described composite expanded liquid is one or more the compound in ethylenediamine tetraacetic methene sodium phosphate, diethanolamine and trolamine, acidity-basicity regulator in described composite expanded liquid is one or both the compound in quadrol and sodium bicarbonate, and the surface tension modifier in described composite expanded liquid is one or more the compound in methyl alcohol, Sodium dodecylbenzene sulfonate, ethanol and ethyl acetate.
In the present embodiment, the experiment proved that, for the graphite intercalation compound of 4 parts of identical amounts, use respectively through the composite expanded liquid expansion process 40min obtained by above-mentioned special parameter, 60min, 100min and 120min, following experimental result can be obtained:
Embodiment 5
A kind of composite expanded liquid, formed by following component Homogeneous phase mixing, the mass percent of each component and each component is: superoxol 60%, complexing of metal ion agent 9%, acidity-basicity regulator 2%, surface tension modifier 4%, and all the other are water.Wherein, the concentration of described superoxol is 30%, complexing of metal ion agent in described composite expanded liquid is one or more the compound in ethylenediamine tetraacetic methene sodium phosphate and trolamine, acidity-basicity regulator in described composite expanded liquid is one or both the compound in quadrol and sodium bicarbonate, and the surface tension modifier in described composite expanded liquid is one or more the compound in methyl alcohol, ethanol and ethyl acetate.
In the present embodiment, the experiment proved that, for the graphite intercalation compound of 4 parts of identical amounts, use respectively through the composite expanded liquid expansion process 40min obtained by above-mentioned special parameter, 60min, 100min and 120min, following experimental result can be obtained:
Claims (6)
1. a composite expanded liquid, it is characterized in that being formed by following component Homogeneous phase mixing, the mass percent of each component and each component is: superoxol 60-90%, complexing of metal ion agent 1-10%, acidity-basicity regulator 1-5%, surface tension modifier 0.5-5%, all the other are water.
2. a kind of composite expanded liquid as claimed in claim 1, it is characterized in that: in described composite expanded liquid, the mass percent of superoxol is 85%, the mass percent of complexing of metal ion agent is 5%, the mass percent of acidity-basicity regulator is 3%, the mass percent of surface tension modifier is 2%, and all the other are water.
3. a kind of composite expanded liquid as claimed in claim 1 or 2, is characterized in that: the concentration of described superoxol is 20-30%.
4. a kind of composite expanded liquid as claimed in claim 1 or 2, is characterized in that: the complexing of metal ion agent in described composite expanded liquid is one or more the compound in Seignette salt, trisodium phosphate, disodium edta, oxalic acid, oxalate, Sunmorl N 60S, ethylenediamine tetraacetic methene sodium phosphate, diethanolamine, trolamine.
5. a kind of composite expanded liquid as claimed in claim 1 or 2, is characterized in that: the acidity-basicity regulator in described composite expanded liquid is one or more the compound in hydrochloric acid, sulfuric acid, phosphoric acid, formic acid, acetic acid, oxalic acid, ammoniacal liquor, sodium hydroxide, potassium hydroxide, quadrol, sodium bicarbonate.
6. a kind of composite expanded liquid as claimed in claim 1 or 2, is characterized in that: the surface tension modifier in described composite expanded liquid is one or more the compound in methyl alcohol, ethanol, propyl alcohol, butanols, ethyl acetate.
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| CN201510186549.9A CN104860301A (en) | 2015-04-20 | 2015-04-20 | Composite inflation liquid |
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| CN201510186549.9A CN104860301A (en) | 2015-04-20 | 2015-04-20 | Composite inflation liquid |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102431999A (en) * | 2011-09-22 | 2012-05-02 | 中国科学院金属研究所 | Method for preparing high-quality graphene |
| CN102569756A (en) * | 2011-12-27 | 2012-07-11 | 上海交通大学 | Preparation method of silicon/graphene nanocomposite material for cathode of lithium ion battery |
| WO2013093519A3 (en) * | 2011-12-22 | 2014-02-06 | Bio Nano Consulting | Carbon nanotube aerogels and xerogels for co2 capture |
| CN104058396A (en) * | 2014-07-14 | 2014-09-24 | 复旦大学 | Method for preparing large-size high-quality graphene with controllable number of layers |
-
2015
- 2015-04-20 CN CN201510186549.9A patent/CN104860301A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102431999A (en) * | 2011-09-22 | 2012-05-02 | 中国科学院金属研究所 | Method for preparing high-quality graphene |
| WO2013093519A3 (en) * | 2011-12-22 | 2014-02-06 | Bio Nano Consulting | Carbon nanotube aerogels and xerogels for co2 capture |
| CN102569756A (en) * | 2011-12-27 | 2012-07-11 | 上海交通大学 | Preparation method of silicon/graphene nanocomposite material for cathode of lithium ion battery |
| CN104058396A (en) * | 2014-07-14 | 2014-09-24 | 复旦大学 | Method for preparing large-size high-quality graphene with controllable number of layers |
Non-Patent Citations (1)
| Title |
|---|
| 郑水林: "《非金属矿物材料》", 31 May 2007, 化学工业出版社 * |
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