CN106744926A - A kind of preparation method of expanded graphite - Google Patents
A kind of preparation method of expanded graphite Download PDFInfo
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- CN106744926A CN106744926A CN201611169344.0A CN201611169344A CN106744926A CN 106744926 A CN106744926 A CN 106744926A CN 201611169344 A CN201611169344 A CN 201611169344A CN 106744926 A CN106744926 A CN 106744926A
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Abstract
The present invention relates to field of new, a kind of preparation method of described expanded graphite comprises the following steps：Configure the first mixed solution, including sodium chlorate, perchloric acid and phosphoric acid；First mixed solution, 20 DEG C~45 DEG C stirring reaction 15min~35min is added to obtain the first mixed system in crystalline flake graphite；Configure the second mixed solution, including potassium permanganate, perchloric acid；Second mixed solution, 20 DEG C~45 DEG C stirring reaction 5min~15min is added to obtain the second mixed system in first mixed system；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~1000 DEG C environment no longer to change, the expanded graphite is obtained.The preparation method of described expanded graphite, not only causes that graphite oxidation more thorough, intercalation is in hgher efficiency, and the expansion multiplying power of the expanded graphite of preparation is up to 500ml/g~700ml/g；And step is simple, can realize successive reaction, with short production cycle, is adapted to industrialized 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 " in machine
Tool field of sealing technology has extremely important status；Expanded graphite field of Environment Protection can as oil absorption material, for waste oil reclaim with
And the microbe carrier in waste water treatment；The graphite radiating plate prepared by expanded graphite turns into the conventional metals materials 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 electrolytic
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：
Configure the first mixed solution, including sodium chlorate, perchloric acid and phosphoric acid；
First mixed solution, 20 DEG C~45 DEG C stirring reaction 15min~35min is added to obtain in crystalline flake graphite
First mixed system；
Configure the second mixed solution, including potassium permanganate, perchloric acid；
Add second mixed solution in first mixed system, 20 DEG C~45 DEG C stirring reaction 5min~
15min, obtains the second mixed system；
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~1000 DEG C environment no longer to change, the expansion stone is obtained
Ink.
Alternatively, in the first mixed system preparation process, the ratio of the crystalline flake graphite and first mixed solution
Example is (2~4) g：(1~8) mL.
Alternatively, in first mixed solution, the ratio of the sodium chlorate, the perchloric acid and described phosphoric acid is (0
~2) g：(1~6) mL：(0~2) mL；Potassium permanganate described in second mixed solution, the perchloric acid ratio for (0~
2)g：(1~6) mL；The ratio of second mixed solution and first mixed solution is 3:4~6:5.
Alternatively, also include：The step of first mixed system is carried out into first time ultrasonic vibration 5min~10min,
Ultrasonic power is 500w~800w.
Alternatively, also include：The step of second mixed system is carried out into second ultrasonic vibration 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, the step of being dried to the head product is also included 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：Configuration first mixes
Solution, including sodium chlorate, perchloric acid and phosphoric acid；First mixed solution, 20 DEG C~45 DEG C stirrings are added in crystalline flake graphite
Reaction 15min~35min, obtains the first mixed system；Configure the second mixed solution, including potassium permanganate, perchloric acid；Described
Second mixed solution, 20 DEG C~45 DEG C stirring reaction 5min~15min is added to obtain the second mixing in first mixed system
System；Second mixed system is filtered to take into solid, and it is neutrality to wash to washing lotion, obtains head product；By the head product
It is placed in calcination to volume in 850 DEG C~1000 DEG C environment no longer to change, obtains the expanded graphite.The system of described expanded graphite
Preparation Method, is prepared by the method for step-by-step oxidation intercalation, and in the first oxidation intercalation step, sodium chlorate in acid condition, is released
Put strong oxidizing property Chlorine Dioxide Gas, collaboration ClO4 -First time oxidation, ClO are carried out to graphite4 -、HClO4、H3PO4、PO4 3-、
ClO3 -、HClO3Multistage intercalation configuration is formed Deng group；In the second oxidation intercalation step, with potassium permanganate as primary oxidant, association
Same ClO4 -Second oxidation is carried out to graphite, again intercalation.Not only so that graphite oxidation more thorough, intercalation is in hgher efficiency, prepare
Expanded graphite expansion multiplying power up to 500ml/g~700ml/g；And step is simple, can realize successive reaction, produce week
Phase is short, 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.
Specific embodiment
In order that the object, technical solutions and advantages of the present invention are clearer, below in conjunction with to embodiment party of the invention
Formula 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%, described phosphorus
Acid concentration is 65wt%, is analyzed pure；It is pure that sodium chlorate, potassium permanganate, hydrogen peroxide are analysis；Water is running water；Crystalline flake graphite, contains
Carbon amounts ＞ 98%.
Embodiment 1
The present embodiment provides a kind of preparation method of expanded graphite, comprises the following steps：
S1, the first mixed solution of configuration, including sodium chlorate, perchloric acid and phosphoric acid；The sodium chlorate, the perchloric acid and institute
The ratio of the phosphoric acid stated is 1g：4mL：1mL；
S2, first mixed solution is added in crystalline flake graphite, under the conditions of 30 DEG C, 100r/min stirring 3min, then
300r/min stirrings 20min obtains the first mixed system.
As one embodiment of the present of invention, in the present embodiment, the ratio of the crystalline flake graphite and first mixed solution
Example is 3g：4mL；The crystalline flake graphite is 30 mesh.
First mixed system is carried out into first time ultrasonic vibration 8min, ultrasonic power is 600w.
S3, the second mixed solution of configuration, including potassium permanganate, perchloric acid；The ratio of the potassium permanganate, the perchloric acid
It is 1g：3mL.
S4, second mixed solution is added in first mixed system, 30 DEG C, 300r/min stirring reactions
10min, obtains the second mixed system；The ratio of second mixed solution and first mixed solution is 1:1.
Second mixed system is carried out into second ultrasonic vibration 8min, ultrasonic power is 1800w.
In second mixed system add volume fraction be 30% hydrogen peroxide, to second mixed system without
Color.
S5, second mixed system is filtered to take solid, and it is neutrality to wash to washing lotion, obtains head product；To described
The step of head product is dried, drying temperature is 50 DEG C, and drying time is 3h.
Used as one embodiment of the present of invention, in the present embodiment, the washing lotion is water.
S6, 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 615ml/g.
As convertible embodiment of the invention, order not limited to this step of the preparation method of the expanded graphite, such as
S2, S3 order can be exchanged, and can realize the purpose of the present invention, belong to protection scope of the present invention.
Embodiment 2
The present embodiment provides a kind of preparation method of expanded graphite, comprises the following steps：
S1, the first mixed solution of configuration, including sodium chlorate, perchloric acid and phosphoric acid；The sodium chlorate, the perchloric acid and institute
The ratio of the phosphoric acid stated is 2g：6mL：0.1mL；
S2, first mixed solution is added in crystalline flake graphite, under the conditions of 20 DEG C, 80r/min stirring 5min, then
350r/min stirrings 10min obtains the first mixed system.
As one embodiment of the present of invention, in the present embodiment, the ratio of the crystalline flake graphite and first mixed solution
Example is 2g：1mL；The crystalline flake graphite is 20 mesh.
First mixed system is carried out into first time ultrasonic vibration 5min, ultrasonic power is 800w.
S3, the second mixed solution of configuration, including potassium permanganate, perchloric acid；The ratio of the potassium permanganate, the perchloric acid
It is 0.1g：6mL.
S4, second mixed solution is added in first mixed system, 20 DEG C, 350r/min stirring reactions
15min, obtains the second mixed system；The ratio of second mixed solution and first mixed solution is 3:4.
Second mixed system is carried out into second ultrasonic vibration 5min, ultrasonic power is 1500w.
In second mixed system add volume fraction be 40% hydrogen peroxide, to second mixed system without
Color.
S5, second mixed system is filtered to take solid, and it is neutrality to wash to washing lotion, obtains head product；To described
The step of head product is dried, drying temperature is 40 DEG C, and drying time is 4h.
Used as one embodiment of the present of invention, in the present embodiment, the washing lotion is water.
S6, 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 560ml/g.
Embodiment 3
The present embodiment provides a kind of preparation method of expanded graphite, comprises the following steps：
S1, the first mixed solution of configuration, including sodium chlorate, perchloric acid and phosphoric acid；The sodium chlorate, the perchloric acid and institute
The ratio of the phosphoric acid stated is 0.1g：1mL：2mL；
S2, first mixed solution is added in crystalline flake graphite, under the conditions of 45 DEG C, 120r/min stirring 1min, then
280r/min stirrings 30min obtains the first mixed system.
As one embodiment of the present of invention, in the present embodiment, the ratio of the crystalline flake graphite and first mixed solution
Example is 1g：2mL；The crystalline flake graphite is 35 mesh.
First mixed system is carried out into first time ultrasonic vibration 10min, ultrasonic power is 500w.
S3, the second mixed solution of configuration, including potassium permanganate, perchloric acid；The ratio of the potassium permanganate, the perchloric acid
It is 2g：1mL.
S4, second mixed solution is added in first mixed system, 45 DEG C, 280r/min stirring reactions
5min, obtains the second mixed system；The ratio of second mixed solution and first mixed solution is 6:5.
Second mixed system is carried out into second ultrasonic vibration 10min, ultrasonic power is 2000w.
In second mixed system add volume fraction be 10% hydrogen peroxide, to second mixed system without
Color.
S5, second mixed system is filtered to take solid, and it is neutrality to wash to washing lotion, obtains head product；To described
The step of head product is dried, drying temperature is 65 DEG C, and drying time is 2h.
Used as one embodiment of the present of invention, in the present embodiment, the washing lotion is water.
S6, the head product is placed in calcination to volume in 1000 DEG C of environment no longer changes, obtain the expanded graphite, pass through
Test, its expansion multiplying power is 580ml/g.
Embodiment 4
The present embodiment provides a kind of preparation method of expanded graphite, comprises the following steps：
S1, the first mixed solution of configuration, including sodium chlorate, perchloric acid and phosphoric acid；The sodium chlorate, the perchloric acid and institute
The ratio of the phosphoric acid stated is 0.1g：1mL：2mL；
S2, first mixed solution is added in crystalline flake graphite, under the conditions of 45 DEG C, 120r/min stirring 1min, then
280r/min stirrings 30min obtains the first mixed system.
As one embodiment of the present of invention, in the present embodiment, the ratio of the crystalline flake graphite and first mixed solution
Example is 1g：2mL；The crystalline flake graphite is 35 mesh.
S3, the second mixed solution of configuration, including potassium permanganate, perchloric acid；The ratio of the potassium permanganate, the perchloric acid
It is 2g：1mL.
S4, second mixed solution is added in first mixed system, 45 DEG C, 280r/min stirring reactions
5min, obtains the second mixed system；The ratio of second mixed solution and first mixed solution is 6:5.
Second mixed system is carried out into second ultrasonic vibration 10min, ultrasonic power is 2000w.
S5, second mixed system is filtered to take solid, and it is neutrality to wash to washing lotion, obtains head product；To described
The step of head product is dried, drying temperature is 65 DEG C, and drying time is 2h.
Used as one embodiment of the present of invention, in the present embodiment, the washing lotion is water.
S6, the head product is placed in calcination to volume in 1000 DEG C of environment no longer changes, obtain the expanded graphite, pass through
Test, its expansion multiplying power is 535ml/g.
Embodiment 5
The present embodiment provides a kind of preparation method of expanded graphite, comprises the following steps：
S1, the first mixed solution of configuration, including sodium chlorate, perchloric acid and phosphoric acid；The sodium chlorate, the perchloric acid and institute
The ratio of the phosphoric acid stated is 0.1g：1mL：2mL；
S2, first mixed solution is added in crystalline flake graphite, under the conditions of 45 DEG C, 120r/min stirring 1min, then
280r/min stirrings 30min obtains the first mixed system.
As one embodiment of the present of invention, in the present embodiment, the ratio of the crystalline flake graphite and first mixed solution
Example is 1g：2mL；The crystalline flake graphite is 30 mesh.
S3, the second mixed solution of configuration, including potassium permanganate, perchloric acid；The ratio of the potassium permanganate, the perchloric acid
It is 2g：1mL.
S4, second mixed solution is added in first mixed system, 45 DEG C, 280r/min stirring reactions
5min, obtains the second mixed system；The ratio of second mixed solution and first mixed solution is 6:5.
In second mixed system add volume fraction be 10% hydrogen peroxide, to second mixed system without
Color.
S5, second mixed system is filtered to take solid, and it is neutrality to wash to washing lotion, obtains head product；To described
The step of head product is dried, drying temperature is 65 DEG C, and drying time is 2h.
Used as one embodiment of the present of invention, in the present embodiment, the washing lotion is water.
S6, the head product is placed in calcination to volume in 1000 DEG C of environment no longer changes, obtain the expanded graphite, pass through
Test, its expansion multiplying power is 490ml/g.
Comparative example
A kind of preparation method of expanded graphite of the present invention, comprises the following steps：
S1, perchloric acid is added in crystalline flake graphite, 30 DEG C, 100r/min stirring 3min, then 300r/min stirring 20min,
Obtain the first mixed system；The crystalline flake graphite particle diameter is 30 mesh, and the ratio of the crystalline flake graphite and the perchloric acid is 3g：
4mL。
S2, configuration mixed solution, including potassium permanganate, perchloric acid；The potassium permanganate, the ratio of the perchloric acid are
1g：3mL.
S3, the mixed solution is added in first mixed system, 30 DEG C, 300r/min stirring reaction 10min are obtained
To the second mixed system；The ratio of second mixed solution and the perchloric acid is 1:1.
In second mixed system add volume fraction be 30% hydrogen peroxide, to second mixed system without
Color.
S4, 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.
S5, 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 230ml/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：
Configure the first mixed solution, including sodium chlorate, perchloric acid and phosphoric acid；
First mixed solution, 20 DEG C~45 DEG C stirring reaction 15min~35min is added to obtain first in crystalline flake graphite
Mixed system；
Configure the second mixed solution, including potassium permanganate, perchloric acid；
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 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~1000 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 ratio of the crystalline flake graphite and first mixed solution is (2~4) g：(1~8) mL.
3. the preparation method of expanded graphite according to claim 1 and 2, it is characterised in that in first mixed solution,
The ratio of the sodium chlorate, the perchloric acid and described phosphoric acid is (0~2) g：(1~6) mL：(0~2) mL；Described second mixes
Close potassium permanganate described in solution, the ratio of the perchloric acid is (0~2) g：(1~6) mL；Second mixed solution and institute
The ratio for stating the first mixed solution is 3:4~6:5.
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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| 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 |
| CN114604869A (en) * | 2022-04-22 | 2022-06-10 | 宁波信远炭材料有限公司 | Antioxidant expanded graphite and preparation method and application thereof |
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| 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 |
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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 |
| CN114604869A (en) * | 2022-04-22 | 2022-06-10 | 宁波信远炭材料有限公司 | Antioxidant expanded graphite and preparation method and application thereof |
| CN114604869B (en) * | 2022-04-22 | 2023-12-15 | 宁波信远炭材料有限公司 | Antioxidant expanded graphite and preparation method and application thereof |
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