CN106672962A - Preparation method of expanded graphite - Google Patents
Preparation method of expanded graphite Download PDFInfo
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- CN106672962A CN106672962A CN201611168822.6A CN201611168822A CN106672962A CN 106672962 A CN106672962 A CN 106672962A CN 201611168822 A CN201611168822 A CN 201611168822A CN 106672962 A CN106672962 A CN 106672962A
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The invention relates to the field of new materials, and particularly provides a preparation method of expanded graphite. The preparation method comprises the following steps: adding a first mixed solution into crystalline flake graphite, and performing stirring reaction at 20-45 DEG C for 15-35 minutes to obtain a first mixed system, wherein the first mixed solution comprises sodium chlorate and perchloric acid; adding a second mixed solution into the first mixed system, and performing stirring reaction at 20-45 DEG C for 5-15 minutes to obtain a second mixed system, wherein the second mixed solution comprises potassium permanganate and perchloric acid; filtering the second mixed system to obtain solids, and washing until a washing solution is neutral to obtain a primary product; and burning the primary product at 850-1100 DEG C until the volume does not change any more to obtain the expanded graphite. According to the preparation method of expanded graphite, the expanded graphite is prepared through a multi-step intercalation method, so that the oxidation is more thorough, the intercalation efficiency is higher, and the expansion multiplying power of the prepared expanded graphite can be up to 500-800 ml/g. The preparation method has the advantages of simple steps and short production cycle, can realize continuous reaction and is suitable for industrial production.
Description
Technical field
The present invention relates to field of new, and in particular to a kind of preparation method of expanded graphite.
Background technology
Expanded graphite as manufacture soft graphite intermediate products, be by natural flake graphite it is oxidized, acidifying intercalation, water
Wash, dry, a kind of loose porous vermiform material obtained from high-temperature process, also known as graphite worm.
Expanded graphite not only has the good characteristics such as native graphite heat-resisting, anti-corrosion, conductive, heat conduction, self lubricity in itself,
The performances such as lightweight, softness, the compressible, resiliency not possessed with native graphite also, therefore, in field of sealing technology, expanded graphite
Material has the performance and purposes more excellent than materials such as asbestos, rubber.
The various bands that are made of expanded graphite, plate, sheet material have been widely used as oil, chemical industry, electric power, metallurgy, machinery, space
The industry fields such as boat, nuclear industry.For example, the flexible graphite article being made of expanded graphite is described as the world " king of sealing ",
Mechanical seal field has extremely important status；Expanded graphite can be reclaimed as oil absorption material in field of Environment Protection for waste oil
And the microbe carrier in waste water treatment；The graphite radiating plate prepared by expanded graphite turns into the conventional metals such as substitution copper, aluminium
The heat radiating material of new generation of material.Additionally, expanded graphite also acts as Medical dressing, catalyst, fixation support and solid electricity
Solution liquid etc..
In the prior art, the preparation method of expanded graphite mainly has two kinds of electrochemical process and chemical oxidation graft process, wherein,
Chemical oxidation graft process is industrial application than wide and comparative maturity method.Traditional chemical oxidation graft process prepares swollen
The method of swollen graphite, typically with the concentrated sulfuric acid as intercalator, Cl2, bichromate, H2O2、HNO3Deng the reaction system for oxidant.
However, it is difficult to successive reaction, production cycle are more long, it is difficult to realize the consecutive production of graphite.
The content of the invention
Therefore, to be solved by this invention is the continuity life that the existing expanded graphite production cycle is long, be difficult to graphite
The problem of product.
In order to solve the above technical problems, the technical solution adopted by the present invention is as follows：
A kind of preparation method of expanded graphite of the present invention, comprises the following steps：
The first mixed solution, 20 DEG C~45 DEG C stirring reaction 15min~35min is added to obtain first in crystalline flake graphite
Mixed system；First mixed solution includes sodium chlorate, perchloric acid；
The second mixed solution, 20 DEG C~45 DEG C stirring reaction 5min~15min is added to obtain in first mixed system
To the second mixed system；Second mixed solution includes potassium permanganate, perchloric acid；
Second mixed system is filtered to take into solid, and it is neutrality to wash to washing lotion, obtains head product；
The head product is placed in into calcination to volume in 850 DEG C~1100 DEG C environment no longer to change, the expansion stone is obtained
Ink.
Alternatively, in the first mixed system preparation process, the crystalline flake graphite, the sodium chlorate, the perchloric acid
The ratio of mixed liquor is (2~4) g：(0~2) g：(1~6) mL.
Alternatively, potassium permanganate described in second mixed solution, the ratio of the perchloric acid are (0~2) g：(1~
6)mL；The ratio of second mixed solution and the crystalline flake graphite is (1~8) mL：(2~4) g.
Alternatively, the preparation method of the expanded graphite also includes：First mixed system is carried out into ultrasound for the first time
The step of concussion 5min~10min, ultrasonic power is 500w~800w.
Alternatively, the preparation method of the expanded graphite also includes：Second mixed system is carried out into second ultrasound
The step of concussion 5min~10min, ultrasonic power is 1500w~2000w.
Alternatively, in the first mixed system preparation process, the whipping step is：80r/min~120r/min is stirred
Mix 0~5min, 280r/min~350r/min stirrings 10min~30min；In the second mixed system preparation process, stirring
Speed is：280r/min~350r/min.
Alternatively, the step of being decolourized to the second hybrid system is also included after second ultrasonic step.
Alternatively, the decolorization process is：It is 10%~40% that volume fraction is added in second mixed system
Hydrogen peroxide, it is colourless to second mixed system.
Alternatively, also including the step of be dried to head product before the calcination step, drying temperature is 40 DEG C~
65 DEG C, drying time is 2h~4h.
Alternatively, the washing lotion is water；The crystalline flake graphite mesh number is not more than 35 mesh.
Above-mentioned technical proposal of the invention has advantages below compared to existing technology：
1st, a kind of preparation method of the expanded graphite described in the embodiment of the present invention, comprises the following steps：In crystalline flake graphite
The first mixed solution, 20 DEG C~45 DEG C stirring reaction 15min~35min is added to obtain the first mixed system；First mixing
Solution includes sodium chlorate, perchloric acid；The second mixed solution, 20 DEG C~45 DEG C stirring reactions are added in first mixed system
5min~15min, obtains the second mixed system；Second mixed solution includes potassium permanganate, perchloric acid；Described second is mixed
Solid filters to take in zoarium system, and it is neutrality to wash to washing lotion, obtains head product；The head product is placed in 850 DEG C~1100 DEG C
Calcination to volume no longer changes in environment, obtains the expanded graphite.The preparation method of described expanded graphite, by substep oxygen
Prepared by the method for changing intercalation, in the first oxidation intercalation step, sodium chlorate in acid condition, discharges strong oxidizing property gas dioxy
Change chlorine, collaboration ClO4 -First time oxidation, ClO are carried out to graphite4 -、HClO4、ClO3 -、HClO3Multistage intercalation knot is formed Deng group
Structure；In the second oxidation intercalation step, with potassium permanganate as primary oxidant, ClO is cooperateed with4 -Second oxidation is carried out to graphite, then
Secondary intercalation.Not only so that graphite oxidation more thorough, intercalation is in hgher efficiency, the expansion multiplying power of the expanded graphite of preparation is up to 500ml/
G~800ml/g；And step is simple, can realize successive reaction, with short production cycle, is adapted to industrialized production.
2nd, the preparation method of a kind of expanded graphite described in the embodiment of the present invention, also including first mixed system is entered
The step of row first time ultrasonic vibration so that the solution in system occurs weak cavitation phenomenon, small cavitation bubble is produced, after explosion
Impulsive force and negative-pressure sucking are produced, promotes the generation of chlorine dioxide, oxidant is fully opened graphite linings, effectively shortened anti-
Between seasonable.
3rd, the preparation method of a kind of expanded graphite described in the embodiment of the present invention, also including second mixed system is entered
The step of second ultrasonic vibration of row so that the solution in system occurs strong cavitation phenomenon, constantly produces small cavitation gas
Bubble, these bubbles are hastily a large amount of under acoustic pressure effect to be produced, and constantly fierce explosion, produces powerful impulsive force and negative pressure
Suction, while the oxidation of graphite is promoted again, enables intercalator relatively to smoothly enter graphite between layers, effectively shortens
Reaction time.
4th, the preparation method of a kind of expanded graphite described in the embodiment of the present invention, the first mixed system preparation process
In, first low rate mixing is uniform so that reactant is fully contacted, then quick stirring, allows reaction fully to carry out.Not only effectively shorten
Reaction time, and avoid the problem that the reactant reaction time caused by the uniform velocity stirring is long, reaction is insufficient.
5th, the preparation method of a kind of expanded graphite described in the embodiment of the present invention, also including decolourize the step of, decolorising agent is
The potassium permanganate reaction of hydrogen peroxide, hydrogen peroxide and excess, generation precipitation MnO2, effectively prevent the environment caused by directly discharge
Harm.
6th, a kind of preparation method of the expanded graphite described in the embodiment of the present invention, raw material not sulfur acid, not only enhances product
The inoxidizability and toughness of product, expand the range of application of product；And, generation treatment cost of waste liquor is low, is effectively saved life
Produce cost.
Brief description of the drawings
In order that present disclosure is more likely to be clearly understood, below according to specific embodiment of the invention and combine
Accompanying drawing, the present invention is further detailed explanation, wherein
Fig. 1 is the scanning electron microscopic picture (25 multiplying power) of the expanded graphite prepared by the embodiment of the present invention 1；
Fig. 2 is the scanning electron microscopic picture (1000 multiplying power) of the expanded graphite prepared by the embodiment of the present invention 1；
Fig. 3 is the Raman test collection of illustrative plates of the expanded graphite prepared by the embodiment of the present invention 1.
Specific embodiment
In order that the object, technical solutions and advantages of the present invention are clearer, below in conjunction with accompanying drawing to reality of the invention
The mode of applying is described in further detail.
The present invention can be embodied in many different forms, and should not be construed as limited to embodiment set forth herein.
Conversely, there is provided these embodiments so that the disclosure will be thorough and complete, and will it is of the invention design be fully conveyed to
Those skilled in the art, the present invention will only be defined by the appended claims.
Compound in following embodiments is commercially available prod, and the concentration of described perchloric acid is 72wt%, is analyzed pure；Chlorine
It is pure that sour sodium, potassium permanganate, hydrogen peroxide are analysis；Water is running water；Crystalline flake graphite, phosphorus content ＞ 98%.
Embodiment 1
The present embodiment provides a kind of preparation method of expanded graphite, comprises the following steps：
S1, the first mixed solution is added in crystalline flake graphite, 30 DEG C, 100r/min stirring reaction 3min, then 300r/min
Stirring reaction 17min, obtains the first mixed system；First mixed solution includes sodium chlorate, perchloric acid；The crystalline flake graphite
It is 30 mesh.
The crystalline flake graphite, the sodium chlorate, the ratio of the perchloric acid mixed liquor are 3g：3g：4mL.
The step of first mixed system is carried out into first time ultrasonic vibration 7min, ultrasonic power is 600w.
S2, the second mixed solution is added in first mixed system, 30 DEG C, 300r/min stirring reaction 10min are obtained
To the second mixed system；Second mixed solution includes potassium permanganate, perchloric acid；
Potassium permanganate described in second mixed solution, the ratio of the perchloric acid are 1g：4mL；Second mixing
The ratio of solution and the crystalline flake graphite is 4mL：3g.
The step of second mixed system is carried out into second ultrasonic vibration 8min, ultrasonic power is 1700w.
In second mixed system add volume fraction be 30% hydrogen peroxide, to second mixed system without
Color.
S3, second mixed system is filtered to take solid, and it is neutrality to wash to washing lotion, obtains head product；To described
Head product is dried, and drying temperature is 50 DEG C, and drying time is 3h.
S4, the head product is placed in calcination to volume in 900 DEG C of environment no longer changes, obtain the expanded graphite, pass through
Test, its expansion multiplying power is 780ml/g.
As shown in Figure 1 and Figure 2, Raman test collection of illustrative plates is as shown in Figure 3 for the scanning electron microscopic picture of the expanded graphite.
Embodiment 2
The present embodiment provides a kind of preparation method of expanded graphite, comprises the following steps：
S1, the first mixed solution is added in crystalline flake graphite, 45 DEG C, 80r/min stirring reaction 3min, then 350r/min are stirred
Reaction 12min is mixed, the first mixed system is obtained；First mixed solution includes sodium chlorate, perchloric acid；The crystalline flake graphite is
35 mesh
The crystalline flake graphite, the sodium chlorate, the ratio of the perchloric acid mixed liquor are 2g：2g：6mL.
The step of first mixed system is carried out into first time ultrasonic vibration 5min, ultrasonic power is 800w.
S2, the second mixed solution is added in first mixed system, 20 DEG C, 350r/min stirring reaction 15min are obtained
To the second mixed system；Second mixed solution includes potassium permanganate, perchloric acid；
Potassium permanganate described in second mixed solution, the ratio of the perchloric acid are 0.1g：6mL；Described second mixes
The ratio for closing solution and the crystalline flake graphite is 1mL：2g.
The step of second mixed system is carried out into second ultrasonic vibration 10min, ultrasonic power is 1500w.
In second mixed system add volume fraction be 10% hydrogen peroxide, to second mixed system without
Color.
S3, second mixed system is filtered to take solid, and it is neutrality to wash to washing lotion, obtains head product；To described
Head product is dried, and drying temperature is 65 DEG C, and drying time is 2h.
S4, the head product is placed in calcination to volume in 850 DEG C of environment no longer changes, obtain the expanded graphite, pass through
Test, its expansion multiplying power is 690ml/g.
Embodiment 3
The present embodiment provides a kind of preparation method of expanded graphite, comprises the following steps：
S1, the first mixed solution is added in crystalline flake graphite, 20 DEG C, 120r/min stirring reaction 1min, then 280r/min
Stirring reaction 34min, obtains the first mixed system；First mixed solution includes sodium chlorate, perchloric acid；The crystalline flake graphite
It is 20 mesh.
The crystalline flake graphite, the sodium chlorate, the ratio of the perchloric acid mixed liquor are 4g：0.1g：1mL.
The step of first mixed system is carried out into first time ultrasonic vibration 10min, ultrasonic power is 500w.
S2, the second mixed solution is added in first mixed system, 45 DEG C, 280r/min stirring reaction 5min are obtained
To the second mixed system；Second mixed solution includes potassium permanganate, perchloric acid；
Potassium permanganate described in second mixed solution, the ratio of the perchloric acid are 2g：1mL；Second mixing
The ratio of solution and the crystalline flake graphite is 8mL：4g.
The step of second mixed system is carried out into second ultrasonic vibration 5min, ultrasonic power is 2000w.
In second mixed system add volume fraction be 40% hydrogen peroxide, to second mixed system without
Color.
S3, second mixed system is filtered to take solid, and it is neutrality to wash to washing lotion, obtains head product；To described
Head product is dried, and drying temperature is 40 DEG C, and drying time is 4h.
S4, the head product is placed in calcination to volume in 1100 DEG C of environment no longer changes, obtain the expanded graphite, pass through
Test, its expansion multiplying power is 750ml/g.
Embodiment 4
The present embodiment provides a kind of preparation method of expanded graphite, comprises the following steps：
S1, the first mixed solution is added in crystalline flake graphite, 30 DEG C, 100r/min stirring reaction 3min, then 300r/min
Stirring reaction 17min, obtains the first mixed system；First mixed solution includes sodium chlorate, perchloric acid；The crystalline flake graphite
It is 30 mesh.
The crystalline flake graphite, the sodium chlorate, the ratio of the perchloric acid mixed liquor are 3g：3g：4mL.
The step of first mixed system is carried out into first time ultrasonic vibration 7min, ultrasonic power is 600w.
S2, the second mixed solution is added in first mixed system, 30 DEG C, 300r/min stirring reaction 10min are obtained
To the second mixed system；Second mixed solution includes potassium permanganate, perchloric acid；
Potassium permanganate described in second mixed solution, the ratio of the perchloric acid are 1g：4mL；Second mixing
The ratio of solution and the crystalline flake graphite is 4mL：3g.
The step of second mixed system is carried out into second ultrasonic vibration 8min, ultrasonic power is 1700w.
S3, second mixed system is filtered to take solid, and it is neutrality to wash to washing lotion, obtains head product；To described
Head product is dried, and drying temperature is 50 DEG C, and drying time is 3h.
S4, the head product is placed in calcination to volume in 900 DEG C of environment no longer changes, obtain the expanded graphite, pass through
Test, its expansion multiplying power is 580ml/g.
Embodiment 5
The present embodiment provides a kind of preparation method of expanded graphite, comprises the following steps：
S1, the first mixed solution is added in crystalline flake graphite, 30 DEG C, 100r/min stirring reaction 3min, then 300r/min
Stirring reaction 17min, obtains the first mixed system；First mixed solution includes sodium chlorate, perchloric acid；The crystalline flake graphite
It is 20 mesh.
The crystalline flake graphite, the sodium chlorate, the ratio of the perchloric acid mixed liquor are 3g：3g：4mL.
S2, the second mixed solution is added in first mixed system, 30 DEG C, 300r/min stirring reaction 10min are obtained
To the second mixed system；Second mixed solution includes potassium permanganate, perchloric acid；
Potassium permanganate described in second mixed solution, the ratio of the perchloric acid are 1g：4mL；Second mixing
The ratio of solution and the crystalline flake graphite is 4mL：3g.
The step of second mixed system is carried out into second ultrasonic vibration 8min, ultrasonic power is 1700w.
In second mixed system add volume fraction be 30% hydrogen peroxide, to second mixed system without
Color.
S3, second mixed system is filtered to take solid, and it is neutrality to wash to washing lotion, obtains head product；To described
Head product is dried, and drying temperature is 50 DEG C, and drying time is 3h.
S4, the head product is placed in calcination to volume in 900 DEG C of environment no longer changes, obtain the expanded graphite, pass through
Test, its expansion multiplying power is 530ml/g.
Embodiment 6
The present embodiment provides a kind of preparation method of expanded graphite, comprises the following steps：
S1, the first mixed solution is added in crystalline flake graphite, 30 DEG C, 100r/min stirring reaction 3min, then 300r/min
Stirring reaction 17min, obtains the first mixed system；First mixed solution includes sodium chlorate, perchloric acid；The crystalline flake graphite
It is 30 mesh.
The crystalline flake graphite, the sodium chlorate, the ratio of the perchloric acid mixed liquor are 3g：3g：4mL.
The step of first mixed system is carried out into first time ultrasonic vibration 7min, ultrasonic power is 600w.
S2, the second mixed solution is added in first mixed system, 30 DEG C, 300r/min stirring reaction 10min are obtained
To the second mixed system；Second mixed solution includes potassium permanganate, perchloric acid；
Potassium permanganate described in second mixed solution, the ratio of the perchloric acid are 1g：4mL；Second mixing
The ratio of solution and the crystalline flake graphite is 4mL：3g.
In second mixed system add volume fraction be 30% hydrogen peroxide, to second mixed system without
Color.
S3, second mixed system is filtered to take solid, and it is neutrality to wash to washing lotion, obtains head product；To described
Head product is dried, and drying temperature is 50 DEG C, and drying time is 3h.
S4, the head product is placed in calcination to volume in 900 DEG C of environment no longer changes, obtain the expanded graphite, pass through
Test, its expansion multiplying power is 620ml/g.
Embodiment 7
The present embodiment provides a kind of preparation method of expanded graphite, comprises the following steps：
S1, the first mixed solution is added in crystalline flake graphite, 30 DEG C, 100r/min stirring reaction 3min, then 300r/min
Stirring reaction 17min, obtains the first mixed system；First mixed solution includes sodium chlorate, perchloric acid；The crystalline flake graphite
It is 30 mesh.
The crystalline flake graphite, the sodium chlorate, the ratio of the perchloric acid mixed liquor are 3g：3g：4mL.
The step of first mixed system is carried out into first time ultrasonic vibration 7min, ultrasonic power is 600w.
S2, the second mixed solution is added in first mixed system, 30 DEG C, 300r/min stirring reaction 10min are obtained
To the second mixed system；Second mixed solution includes potassium permanganate, perchloric acid；
Potassium permanganate described in second mixed solution, the ratio of the perchloric acid are 1g：4mL；Second mixing
The ratio of solution and the crystalline flake graphite is 4mL：3g.
The step of second mixed system is carried out into second ultrasonic vibration 8min, ultrasonic power is 1700w.
In second mixed system add volume fraction be 30% hydrogen peroxide, to second mixed system without
Color.
S3, second mixed system is filtered to take solid, and it is neutrality to wash to washing lotion, obtains head product.
S4, the head product is placed in calcination to volume in 900 DEG C of environment no longer changes, obtain the expanded graphite, pass through
Test, its expansion multiplying power is 610ml/g.
Embodiment 8
The present embodiment provides a kind of preparation method of expanded graphite, comprises the following steps：
S1, the first mixed solution is added in crystalline flake graphite, 30 DEG C, 100r/min stirring reaction 3min, then 300r/min
Stirring reaction 17min, obtains the first mixed system；First mixed solution includes sodium chlorate, perchloric acid；The crystalline flake graphite
It is 30 mesh.
The crystalline flake graphite, the sodium chlorate, the ratio of the perchloric acid mixed liquor are 3g：3g：4mL.
S2, the second mixed solution is added in first mixed system, 30 DEG C, 300r/min stirring reaction 10min are obtained
To the second mixed system；Second mixed solution includes potassium permanganate, perchloric acid；
Potassium permanganate described in second mixed solution, the ratio of the perchloric acid are 1g：4mL；Second mixing
The ratio of solution and the crystalline flake graphite is 4mL：3g.
S3, second mixed system is filtered to take solid, and it is neutrality to wash to washing lotion, obtains head product.
S4, the head product is placed in calcination to volume in 900 DEG C of environment no longer changes, obtain the expanded graphite, pass through
Test, its expansion multiplying power is 500ml/g.
Comparative example
The present embodiment provides a kind of preparation method of expanded graphite, comprises the following steps：
S1, the first mixed solution is added in crystalline flake graphite, 30 DEG C, 100r/min stirring reaction 20min obtain first and mix
Zoarium system；First mixed solution includes perchloric acid；The crystalline flake graphite is 50 mesh.
The crystalline flake graphite, the ratio of the perchloric acid mixed liquor are 1g：7mL.
S2, the second mixed solution is added in first mixed system, 30 DEG C, 300r/min stirring reaction 10min are obtained
To the second mixed system；Second mixed solution includes potassium permanganate, perchloric acid；
Potassium permanganate described in second mixed solution, the ratio of the perchloric acid are 1g：4mL；Second mixing
The ratio of solution and the crystalline flake graphite is 4mL：3g.
S3, second mixed system is filtered to take solid, and it is neutrality to wash to washing lotion, obtains head product.
S4, the head product is placed in calcination to volume in 900 DEG C of environment no longer changes, obtain the expanded graphite, pass through
Test, its expansion multiplying power is 200ml/g.
Obviously, above-described embodiment is only intended to clearly illustrate example, and not to the restriction of implementation method.It is right
For those of ordinary skill in the art, can also make on the basis of the above description other multi-forms change or
Change.There is no need and unable to be exhaustive to all of implementation method.And the obvious change thus extended out or
Among changing still in protection scope of the present invention.
Claims (10)
1. a kind of preparation method of expanded graphite, it is characterised in that comprise the following steps：
The first mixed solution, 20 DEG C~45 DEG C stirring reaction 15min~35min is added to obtain the first mixing in crystalline flake graphite
System；First mixed solution includes sodium chlorate, perchloric acid；
The second mixed solution, 20 DEG C~45 DEG C stirring reaction 5min~15min is added to obtain in first mixed system
Two mixed systems；Second mixed solution includes potassium permanganate, perchloric acid；
Second mixed system is filtered to take into solid, and it is neutrality to wash to washing lotion, obtains head product；
The head product is placed in into calcination to volume in 850 DEG C~1100 DEG C environment no longer to change, the expanded graphite is obtained.
2. the preparation method of expanded graphite according to claim 1, it is characterised in that first mixed system prepares step
In rapid, the crystalline flake graphite, the sodium chlorate, the ratio of the perchloric acid mixed liquor are (2~4) g：(0~2) g：(1~6)
mL。
3. the preparation method of expanded graphite according to claim 1 and 2, it is characterised in that in second mixed solution
The potassium permanganate, the ratio of the perchloric acid are (0~2) g：(1~6) mL；Second mixed solution and the scale stone
The ratio of ink is (1~8) mL：(2~4) g.
4. the preparation method of the expanded graphite according to claim any one of 1-3, it is characterised in that also include：Will be described
The step of first mixed system carries out first time ultrasonic vibration 5min~10min, ultrasonic power is 500w~800w.
5. the preparation method of the expanded graphite according to claim any one of 1-4, it is characterised in that also include：Will be described
The step of second mixed system carries out second ultrasonic vibration 5min~10min, ultrasonic power is 1500w~2000w.
6. the preparation method of the expanded graphite according to claim any one of 1-5, it is characterised in that first mixture
It is that the whipping step is in preparation process：80r/min~120r/min stirs 0~5min, and 280r/min~350r/min is stirred
Mix 10min~30min；In the second mixed system preparation process, mixing speed is：280r/min~350r/min.
7. the preparation method of the expanded graphite according to claim 5 or 6, it is characterised in that second ultrasonic step
Also include the step of being decolourized to the second hybrid system afterwards.
8. the preparation method of expanded graphite according to claim 7, it is characterised in that the decolorization process is：Described
The hydrogen peroxide that volume fraction is 10%~40% is added in second mixed system, it is colourless to second mixed system.
9. the preparation method of the expanded graphite according to claim any one of 1-8, it is characterised in that the calcination step it
Preceding also to include the step of being dried to the head product, drying temperature is 40 DEG C~65 DEG C, and drying time is 2h~4h.
10. the preparation method of the expanded graphite according to claim any one of 1-9, it is characterised in that the washing lotion is water；
The crystalline flake graphite mesh number is not more than 35 mesh.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110104633A (en) * | 2019-04-27 | 2019-08-09 | 北京鼎臣石墨科技有限公司 | A kind of preparation method of graphene oxide and graphene |
| CN113735113A (en) * | 2021-10-21 | 2021-12-03 | 青岛洛唯新材料有限公司 | Expandable graphite and preparation method thereof |
| CN116397122A (en) * | 2023-04-07 | 2023-07-07 | 长春工业大学 | Nickel-plated expanded graphite-Cu composite material and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102320596A (en) * | 2011-07-13 | 2012-01-18 | 武汉理工大学 | Preparation method of fine-flake expanded graphite |
| CN104401978A (en) * | 2014-10-30 | 2015-03-11 | 宜昌新成石墨有限责任公司 | Preparation method for sulfur-free expandable graphite |
| CN104828818A (en) * | 2015-05-27 | 2015-08-12 | 北京鼎臣超导科技有限公司 | Efficient intercalation stripping method of micrometer graphite flakes and low-order graphite intercalation compounds and micrometer thin-wall porous expanded graphite |
-
2016
- 2016-12-16 CN CN201611168822.6A patent/CN106672962A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102320596A (en) * | 2011-07-13 | 2012-01-18 | 武汉理工大学 | Preparation method of fine-flake expanded graphite |
| CN104401978A (en) * | 2014-10-30 | 2015-03-11 | 宜昌新成石墨有限责任公司 | Preparation method for sulfur-free expandable graphite |
| CN104828818A (en) * | 2015-05-27 | 2015-08-12 | 北京鼎臣超导科技有限公司 | Efficient intercalation stripping method of micrometer graphite flakes and low-order graphite intercalation compounds and micrometer thin-wall porous expanded graphite |
Non-Patent Citations (1)
| Title |
|---|
| 周丹凤: "低温可膨胀石墨的制备研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110104633A (en) * | 2019-04-27 | 2019-08-09 | 北京鼎臣石墨科技有限公司 | A kind of preparation method of graphene oxide and graphene |
| CN113735113A (en) * | 2021-10-21 | 2021-12-03 | 青岛洛唯新材料有限公司 | Expandable graphite and preparation method thereof |
| CN116397122A (en) * | 2023-04-07 | 2023-07-07 | 长春工业大学 | Nickel-plated expanded graphite-Cu composite material and preparation method and application thereof |
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