CN106698413A - Method for preparing expandable graphite - Google Patents
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Abstract
The invention relates to the field of new materials and provides a method for preparing expandable graphite. The method comprises the following steps: preparing a first mixture solution containing sodium chlorate and perchloric acid; adding the first mixture solution into scale graphite, and carrying out a reaction for 15 to 35 minutes at the temperature of 20 DEG C to 45 DEG C with stirring, so as to obtain a first mixture system; preparing a second mixture solution containing potassium permanganate, perchloric acid and phosphoric acid; adding the second mixture solution into the first mixture system, and carrying out a reaction for 5 to 15 minutes at the temperature of 20 DEG C to 45 DEG C with stirring, so as to obtain a second mixture system; filtering the second mixture system to obtain solids, and washing the solids until washing liquid is neutral, so as to obtain a primary product; burning the primary product in an environment with the temperature of 850 DEG C to 1,000 DEG C until the volume does not change any more, thereby obtaining the expandable graphite. According to the method for preparing the expandable graphite, the graphite oxidation is more thorough, the intercalation efficiency is higher, and the expansion multiplying factor of the prepared expandable graphite can reach 500ml/g to 700ml/g; the steps are simple, continuous reaction can be achieved, and the production cycle is short, so that the method is applicable to 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 " 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；
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 and phosphoric 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：(1~6) mL.
Alternatively, the ratio of sodium chlorate and the perchloric acid described in first mixed solution is (0~2) g：(1~6)
mL；The ratio of potassium permanganate, the perchloric acid and described phosphoric acid described in second mixed solution is (0~2) g：(1~
6)mL：(0~2) mL；The ratio of second mixed solution and first mixed solution is 4:5~6:5.
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 mixed 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；First mixed solution, 20 DEG C~45 DEG C stirring reactions are added in crystalline flake graphite
15min~35min, obtains the first mixed system；Configure the second mixed solution, including potassium permanganate, perchloric acid and phosphoric acid；Institute
State and add in the first mixed system second mixed solution, 20 DEG C~45 DEG C stirring reaction 5min~15min obtain second and mix
Zoarium system；Second mixed system is filtered to take into solid, and it is neutrality to wash to washing lotion, obtains head product；By the primiparity
Thing is placed in calcination to volume in 850 DEG C~1000 DEG C environment no longer to be changed, and obtains the expanded graphite.Described expanded graphite
Preparation method, is prepared by the method for step-by-step oxidation intercalation, in the first oxidation intercalation step, sodium chlorate in acid condition,
Release strong oxidizing property Chlorine Dioxide Gas, collaboration ClO4 -First time oxidation, ClO are carried out to graphite4 -、HClO4、ClO3 -、HClO3Deng
Group forms multistage intercalation configuration；In the second oxidation intercalation step, with potassium permanganate as primary oxidant, ClO is cooperateed with4 -To graphite
Carry out second oxidation, H3PO4、PO4 3-Intercalation effect is enhanced again Deng group.Not only so that graphite oxidation more thorough, intercalation
In hgher efficiency, the expansion multiplying power of the expanded graphite of preparation is up to 500ml/g~700ml/g；And step it is simple, being capable of the company of realization
Continuous reaction, with short production cycle, suitable 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 flow chart of the preparation method of the expanded graphite described in 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%, 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 preparation method of a kind of expanded graphite of the present invention, as shown in figure 1, comprising the following steps：
The ratio of S1, the first mixed solution of configuration, including sodium chlorate, perchloric acid, the sodium chlorate and the perchloric acid is
0.1g：6mL.
S2, first mixed solution is added in crystalline flake graphite, 30 DEG C, 100r/min stirring 3min, then 300r/min
Stirring 20min, obtains the first mixed system；The crystalline flake graphite particle diameter is 30 mesh, and the crystalline flake graphite mixes with described first
The ratio of solution is 3g：4mL.
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 and phosphoric acid；Described in second mixed solution
The ratio of potassium permanganate, the perchloric acid and described phosphoric acid is 1g：3mL：1mL.
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
Head product is dried, and drying temperature is 50 DEG C, and drying time is 3h.
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 630ml/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
A kind of preparation method of expanded graphite of the present invention, comprises the following steps：
The ratio of S1, the first mixed solution of configuration, including sodium chlorate, perchloric acid, the sodium chlorate and the perchloric acid is
2g：4mL.
S2, first mixed solution is added in crystalline flake graphite, 20 DEG C, 80r/min stirring 5min, then 280r/min is stirred
30min is mixed, the first mixed system is obtained；The crystalline flake graphite particle diameter is 20 mesh, and the crystalline flake graphite mixes molten with described first
The ratio of liquid is 2g：1mL.
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 and phosphoric acid；Described in second mixed solution
The ratio of potassium permanganate, the perchloric acid and described phosphoric acid is 2g：6mL：0.1mL.
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 4:5.
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.
S5, 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 2h.
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 600ml/g.
Embodiment 3
A kind of preparation method of expanded graphite of the present invention, comprises the following steps：
The ratio of S1, the first mixed solution of configuration, including sodium chlorate, perchloric acid, the sodium chlorate and the perchloric acid is
1g：1mL.
S2, first mixed solution is added in crystalline flake graphite, 45 DEG C, 120r/min stirring 1min, then 350r/min
Stirring 10min, obtains the first mixed system；The crystalline flake graphite particle diameter is 35 mesh, and the crystalline flake graphite mixes with described first
The ratio of solution is 2g：3mL.
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 and phosphoric acid；Described in second mixed solution
The ratio of potassium permanganate, the perchloric acid and described phosphoric acid is 0.1g：1mL：2mL.
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 1500w.
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
Head product is dried, and drying temperature is 65 DEG C, and drying time is 4h.
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 590ml/g.
Embodiment 4
A kind of preparation method of expanded graphite of the present invention, comprises the following steps：
The ratio of S1, the first mixed solution of configuration, including sodium chlorate, perchloric acid, the sodium chlorate and the perchloric acid is
0.1g：6mL.
S2, first mixed solution is added in crystalline flake graphite, 30 DEG C, 100r/min stirring 1min, then 300r/min
Stirring 19min, obtains the first mixed system；The crystalline flake graphite particle diameter is 30 mesh, and the crystalline flake graphite mixes with described first
The ratio of solution is 3g：4mL.
S3, the second mixed solution of configuration, including potassium permanganate, perchloric acid and phosphoric acid；Described in second mixed solution
The ratio of potassium permanganate, the perchloric acid and described phosphoric acid is 1g：3mL：1mL.
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
Head product is dried, and drying temperature is 50 DEG C, and drying time is 3h.
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 600ml/g.
Embodiment 5
A kind of preparation method of expanded graphite of the present invention, comprises the following steps：
The ratio of S1, the first mixed solution of configuration, including sodium chlorate, perchloric acid, the sodium chlorate and the perchloric acid is
0.1g：6mL.
S2, first mixed solution is added in crystalline flake graphite, 30 DEG C, 100r/min stirring 3min, then 300r/min
Stirring 20min, obtains the first mixed system；The crystalline flake graphite particle diameter is 20 mesh, and the crystalline flake graphite mixes with described first
The ratio of solution is 3g：4mL.
S3, the second mixed solution of configuration, including potassium permanganate, perchloric acid and phosphoric acid；Described in second mixed solution
The ratio of potassium permanganate, the perchloric acid and described phosphoric acid is 1g：3mL：1mL.
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.
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
Head product is dried, and drying temperature is 50 DEG C, and drying time is 3h.
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 490ml/g.
Embodiment 6
A kind of preparation method of expanded graphite of the present invention, comprises the following steps：
The ratio of S1, the first mixed solution of configuration, including sodium chlorate, perchloric acid, the sodium chlorate and the perchloric acid is
0.1g：6mL；
S2, first mixed solution is added in crystalline flake graphite, 30 DEG C, 100r/min stirring 3min, then 300r/min
Stirring 20min, obtains the first mixed system；The crystalline flake graphite particle diameter is 30 mesh, and the crystalline flake graphite mixes with described first
The ratio of solution is 3g：4mL.
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 and phosphoric acid；Described in second mixed solution
The ratio of potassium permanganate, the perchloric acid and described phosphoric acid is 1g：3mL：1mL.
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.
S5, 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.
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 610ml/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；
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 and phosphoric 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：(1~6) 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 and the perchloric acid is (0~2) g：(1~6) mL；Permanganic acid described in second mixed solution
The ratio of potassium, the perchloric acid and described phosphoric acid is (0~2) g：(1~6) mL：(0~2) mL；Second mixed solution with
The ratio of first mixed solution is 4:5~5:6.
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 mixed 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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| CN105347339A (en) * | 2015-12-11 | 2016-02-24 | 中国科学院兰州化学物理研究所 | Preparation method of expanded graphite |
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| 吕广超等: "以高氯酸和磷酸为插层剂制备无硫可膨胀石墨的研究", 《黑龙江科学》 * |
| 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》 * |
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