CN106744926B - A kind of preparation method of expanded graphite - Google Patents
A kind of preparation method of expanded graphite Download PDFInfo
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Abstract
The present invention relates to field of new materials, a kind of preparation method of expanded graphite includes the following steps: to configure the first mixed solution, including sodium chlorate, perchloric acid and phosphoric acid；First mixed solution is added in crystalline flake graphite, 20 DEG C~45 DEG C are stirred to react 15min~35min, obtain the first mixed system；Configure the second mixed solution, including potassium permanganate, perchloric acid；Second mixed solution is added in first mixed system, 20 DEG C~45 DEG C are stirred to react 5min~15min, obtain the second mixed system；Second mixed system is filtered to take into solid, and washing to washing lotion is neutrality, obtains head product；The head product is placed in 850 DEG C~1000 DEG C environment calcination no longer to change to volume, obtains the expanded graphite.The preparation method of the expanded graphite, not only make graphite oxidation more thoroughly, intercalation it is more efficient, the expansion multiplying power of the expanded graphite of preparation is up to 500ml/g~700ml/g；And step is simple, can be realized successive reaction, is with short production cycle, is suitble to industrialized production.
Description
Technical field
The present invention relates to field of new materials, and in particular to a kind of preparation method of expanded graphite.
Background technique
Intermediate products of the expanded graphite as manufacture soft graphite, are to be aoxidized by natural flake graphite, be acidified intercalation, water
It washes, dry, the vermiform substance also known as graphite worm that one kind obtained from high-temperature process is loose porous.
Expanded graphite not only has the good characteristics such as the heat-resisting, anti-corrosion, conductive, thermally conductive of natural graphite itself, self-lubrication,
The performances such as the lightweight that does not have with natural graphite also, softness, compressible, resilient, therefore, in field of sealing technology, expanded graphite
Material has performance more superior than materials such as asbestos, rubber and purposes.
The various bands made of expanded graphite, plate, sheet material have been widely used as petroleum, chemical industry, electric power, metallurgy, machinery, space
The industry fields such as boat, nuclear industry.For example, the flexible graphite article made of expanded graphite is known as the world " king of sealing " in machine
Tool field of sealing technology has extremely important status；Expanded graphite can be used as oil absorption material in environment protection field, for waste oil recycle with
And the microbe carrier in waste water treatment；Become by the graphite radiating plate of expanded graphite preparation and replaces the conventional metals materials such as copper, aluminium
The heat radiating material of new generation of material.In addition, 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 electrochemical process and two kinds of 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, generally using the concentrated sulfuric acid as intercalator, Cl2, bichromate, H2O2、HNO3Deng the reaction system for oxidant.
However, it is difficult to which successive reaction, production cycle are longer, it is difficult to realize the consecutive production of graphite.
Summary of the invention
For this purpose, to be solved by this invention is the continuity life that the existing expanded graphite production cycle is long, is difficult to realize graphite
The problem of production.
In order to solve the above technical problems, The technical solution adopted by the invention is as follows:
A kind of preparation method of expanded graphite of the present invention, includes the following steps:
Configure the first mixed solution, including sodium chlorate, perchloric acid and phosphoric acid；
First mixed solution is added in crystalline flake graphite, 20 DEG C~45 DEG C are stirred to react 15min~35min, obtain
First mixed system；
Configure the second mixed solution, including potassium permanganate, perchloric acid；
Be added second mixed solution in first mixed system, 20 DEG C~45 DEG C be stirred to react 5min~
15min obtains the second mixed system；
Second mixed system is filtered to take into solid, and washing to washing lotion is neutrality, obtains head product；
The head product is placed in 850 DEG C~1000 DEG C environment calcination no longer to change to volume, obtains the expansion stone
Ink.
Optionally, in the first mixed system preparation step, the ratio of the crystalline flake graphite and first mixed solution
Example is (2~4) g:(1~8) mL.
Optionally, in first mixed solution, the ratio of the sodium chlorate, the perchloric acid and the phosphoric acid is (0
~2) g:(1~6) mL:(0~2) mL；Potassium permanganate described in second mixed solution, the perchloric acid ratio be (0~
2) g:(1~6) mL；The ratio of second mixed solution and first mixed solution is 3:4~6:5.
Optionally, further includes: the step of first mixed system is subjected to first time ultrasonic vibration 5min~10min,
Ultrasonic power is 500w~800w.
Optionally, further includes: the step of second mixed system is subjected to second of ultrasonic vibration 5min~10min,
Ultrasonic power is 1500w~2000w.
Optionally, in the first mixed system preparation step, the whipping step are as follows: 80r/min~120r/min is stirred
0~5min is mixed, 280r/min~350r/min stirs 10min~30min；In the second mixed system preparation step, stirring
Speed are as follows: 280r/min~350r/min.
Optionally, further include the steps that decolourizing to the second hybrid system after second of ultrasonic step.
Optionally, the decolorization process are as follows: it is 10%~40% that volume fraction is added in second mixed system
Hydrogen peroxide, until second mixed system is colourless.
Optionally, before the calcination step further include the steps that the head product is dried, drying temperature 40
DEG C~65 DEG C, drying time is 2h~4h.
Optionally, the washing lotion is water；The crystalline flake graphite mesh number is not more than 35 mesh.
The above technical solution of the present invention has the following advantages over the prior art:
1, a kind of preparation method of expanded graphite described in the embodiment of the present invention includes the following steps: the first mixing of configuration
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
15min~35min is reacted, the first mixed system is obtained；Configure the second mixed solution, including potassium permanganate, perchloric acid；Described
Second mixed solution is added in first mixed system, 20 DEG C~45 DEG C are stirred to react 5min~15min, obtain the second mixing
System；Second mixed system is filtered to take into solid, and washing to washing lotion is neutrality, obtains head product；By the head product
It is placed in calcination in 850 DEG C~1000 DEG C environment no longer to change to volume, obtains the expanded graphite.The system of the 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 -、HClO3Equal groups form multistage intercalation configuration；In the second oxidation intercalation step, using potassium permanganate as main oxidant, association
Same ClO4 -It carries out second to graphite to aoxidize, again intercalation.Not only make graphite oxidation more thoroughly, intercalation it is more efficient, preparation
Expanded graphite expansion multiplying power up to 500ml/g~700ml/g；And step is simple, can be realized successive reaction, production week
Phase is short, is suitble to industrialized production.
2, a kind of preparation method of expanded graphite described in the embodiment of the present invention, further include by first mixed system into
The step of row first time ultrasonic vibration, generates small cavitation bubble, after explosion so that weak cavitation phenomenon occurs for the solution in system
Impact force and negative-pressure sucking are generated, promotes the generation of chlorine dioxide, oxidant is made fully to open graphite linings, is effectively shortened anti-
Between seasonable.
3, a kind of preparation method of expanded graphite described in the embodiment of the present invention, further include by second mixed system into
The step of second of ultrasonic vibration of row, constantly generates small cavitation gas so that strong cavitation phenomenon occurs for the solution in system
Bubble, these bubbles are hastily a large amount of under acoustic pressure effect to be generated, and constantly fierce explosion, generates powerful impact force and negative pressure
Suction enables intercalator relatively to smoothly enter graphite between layers, effectively shortens while promoting the oxidation of graphite again
Reaction time.
4, a kind of preparation method of expanded graphite described in the embodiment of the present invention, the first mixed system preparation step
In, it first mixes slowly uniformly, so that reactant comes into full contact with, then quickly stirring, reaction is allowed sufficiently to carry out.Not only effectively shorten
Reaction time, and avoid because the reactant reaction time is long caused by the uniform velocity stirring, reacts insufficient problem.
5, a kind of preparation method of expanded graphite described in the embodiment of the present invention, further includes the steps that decoloration, and decolorising agent is
Hydrogen peroxide, hydrogen peroxide and the reaction of excessive potassium permanganate, generate precipitating MnO2, environment caused by effectively preventing because of direct emission
Harm.
6, a kind of preparation method of expanded graphite described in the embodiment of the present invention, raw material not sulfur acid, not only enhances production
The inoxidizability and toughness of product, expand the application range of product；Moreover, generation treatment cost of waste liquor is low, it is effectively saved life
Produce cost.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention 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.
On the contrary, providing these embodiments, so that the disclosure will be thorough and complete, and design of the invention will 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 commercial product, and the concentration of the perchloric acid is 72wt%, the phosphorus
Acid concentration is 65wt%, is analyzed pure；Sodium chlorate, potassium permanganate, hydrogen peroxide are that analysis is pure；Water is tap water；Crystalline flake graphite contains
Carbon amounts > 98%.
Embodiment 1
The present embodiment provides a kind of preparation methods of expanded graphite, include 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 for the phosphoric acid stated is 1g:4mL:1mL；
S2, it is added first mixed solution in crystalline flake graphite, under the conditions of 30 DEG C, 100r/min stirs 3min, then
300r/min stirring 20min obtains the first mixed system.
As an embodiment of the present 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 subjected to first time ultrasonic vibration 8min, ultrasonic power 600w.
S3, the second mixed solution of configuration, including potassium permanganate, perchloric acid；The ratio of the potassium permanganate, the perchloric acid
For 1g:3mL.
S4, it is added second mixed solution in first mixed system, 30 DEG C, 300r/min is stirred to react
10min obtains the second mixed system；The ratio of second mixed solution and first mixed solution is 1:1.
Second mixed system is subjected to second of ultrasonic vibration 8min, ultrasonic power 1800w.
In second mixed system be added volume fraction be 30% hydrogen peroxide, until second mixed system without
Color.
S5, second mixed system is filtered to take to solid, and washing to washing lotion is neutrality, obtains head product；To described
The step of head product is dried, drying temperature are 50 DEG C, drying time 3h.
As an embodiment of the present invention, in the present embodiment, the washing lotion is water.
S6, the head product is placed in calcination in 900 DEG C of environment no longer changes to volume, obtain the expanded graphite, pass through
Test, expansion multiplying power 615ml/g.
As convertible embodiment of the invention, sequence is without being limited thereto the step of the preparation method of the expanded graphite, such as
S2, S3 sequence can exchange, and the purpose of the present invention may be implemented, belong to the scope of protection of the present invention.
Embodiment 2
The present embodiment provides a kind of preparation methods of expanded graphite, include 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 for the phosphoric acid stated is 2g:6mL:0.1mL；
S2, it is added first mixed solution in crystalline flake graphite, under the conditions of 20 DEG C, 80r/min stirs 5min, then
350r/min stirring 10min obtains the first mixed system.
As an embodiment of the present 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 subjected to first time ultrasonic vibration 5min, ultrasonic power 800w.
S3, the second mixed solution of configuration, including potassium permanganate, perchloric acid；The ratio of the potassium permanganate, the perchloric acid
For 0.1g:6mL.
S4, it is added second mixed solution in first mixed system, 20 DEG C, 350r/min is stirred to react
15min obtains the second mixed system；The ratio of second mixed solution and first mixed solution is 3:4.
Second mixed system is subjected to second of ultrasonic vibration 5min, ultrasonic power 1500w.
In second mixed system be added volume fraction be 40% hydrogen peroxide, until second mixed system without
Color.
S5, second mixed system is filtered to take to solid, and washing to washing lotion is neutrality, obtains head product；To described
The step of head product is dried, drying temperature are 40 DEG C, drying time 4h.
As an embodiment of the present invention, in the present embodiment, the washing lotion is water.
S6, the head product is placed in calcination in 850 DEG C of environment no longer changes to volume, obtain the expanded graphite, pass through
Test, expansion multiplying power 560ml/g.
Embodiment 3
The present embodiment provides a kind of preparation methods of expanded graphite, include 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 for the phosphoric acid stated is 0.1g:1mL:2mL；
S2, it is added first mixed solution in crystalline flake graphite, under the conditions of 45 DEG C, 120r/min stirs 1min, then
280r/min stirring 30min obtains the first mixed system.
As an embodiment of the present 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 subjected to first time ultrasonic vibration 10min, ultrasonic power 500w.
S3, the second mixed solution of configuration, including potassium permanganate, perchloric acid；The ratio of the potassium permanganate, the perchloric acid
For 2g:1mL.
S4, it is added second mixed solution in first mixed system, 45 DEG C, 280r/min is stirred to react
5min obtains the second mixed system；The ratio of second mixed solution and first mixed solution is 6:5.
Second mixed system is subjected to second of ultrasonic vibration 10min, ultrasonic power 2000w.
In second mixed system be added volume fraction be 10% hydrogen peroxide, until second mixed system without
Color.
S5, second mixed system is filtered to take to solid, and washing to washing lotion is neutrality, obtains head product；To described
The step of head product is dried, drying temperature are 65 DEG C, drying time 2h.
As an embodiment of the present invention, in the present embodiment, the washing lotion is water.
S6, the head product is placed in calcination in 1000 DEG C of environment no longer changes to volume, obtain the expanded graphite, pass through
Test, expansion multiplying power 580ml/g.
Embodiment 4
The present embodiment provides a kind of preparation methods of expanded graphite, include 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 for the phosphoric acid stated is 0.1g:1mL:2mL；
S2, it is added first mixed solution in crystalline flake graphite, under the conditions of 45 DEG C, 120r/min stirs 1min, then
280r/min stirring 30min obtains the first mixed system.
As an embodiment of the present 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
For 2g:1mL.
S4, it is added second mixed solution in first mixed system, 45 DEG C, 280r/min is stirred to react
5min obtains the second mixed system；The ratio of second mixed solution and first mixed solution is 6:5.
Second mixed system is subjected to second of ultrasonic vibration 10min, ultrasonic power 2000w.
S5, second mixed system is filtered to take to solid, and washing to washing lotion is neutrality, obtains head product；To described
The step of head product is dried, drying temperature are 65 DEG C, drying time 2h.
As an embodiment of the present invention, in the present embodiment, the washing lotion is water.
S6, the head product is placed in calcination in 1000 DEG C of environment no longer changes to volume, obtain the expanded graphite, pass through
Test, expansion multiplying power 535ml/g.
Embodiment 5
The present embodiment provides a kind of preparation methods of expanded graphite, include 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 for the phosphoric acid stated is 0.1g:1mL:2mL；
S2, it is added first mixed solution in crystalline flake graphite, under the conditions of 45 DEG C, 120r/min stirs 1min, then
280r/min stirring 30min obtains the first mixed system.
As an embodiment of the present 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
For 2g:1mL.
S4, it is added second mixed solution in first mixed system, 45 DEG C, 280r/min is stirred to react
5min obtains the second mixed system；The ratio of second mixed solution and first mixed solution is 6:5.
In second mixed system be added volume fraction be 10% hydrogen peroxide, until second mixed system without
Color.
S5, second mixed system is filtered to take to solid, and washing to washing lotion is neutrality, obtains head product；To described
The step of head product is dried, drying temperature are 65 DEG C, drying time 2h.
As an embodiment of the present invention, in the present embodiment, the washing lotion is water.
S6, the head product is placed in calcination in 1000 DEG C of environment no longer changes to volume, obtain the expanded graphite, pass through
Test, expansion multiplying power 490ml/g.
Comparative example
A kind of preparation method of expanded graphite of the present invention, includes the following steps:
S1, perchloric acid is added in crystalline flake graphite, 30 DEG C, 100r/min stirs 3min, then 300r/min stirs 20min,
Obtain the first mixed system；The crystalline flake graphite partial size 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 perchloric acid ratio be
1g:3mL.
S3, be added the mixed solution in first mixed system, 30 DEG C, 300r/min be stirred to react 10min, obtain
To the second mixed system；The ratio of second mixed solution and the perchloric acid is 1:1.
In second mixed system be added volume fraction be 30% hydrogen peroxide, until second mixed system without
Color.
S4, second mixed system is filtered to take to solid, and washing to washing lotion is neutrality, obtains head product；To described
Head product is dried, and drying temperature is 50 DEG C, drying time 3h.
S5, the head product is placed in calcination in 900 DEG C of environment no longer changes to volume, obtain the expanded graphite, pass through
Test, expansion multiplying power 230ml/g.
Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And it is extended from this it is obvious variation or
Variation is still in the protection scope of this invention.
Claims (8)
1. a kind of preparation method of expanded graphite, which comprises the steps of:
Configure the first mixed solution, including sodium chlorate, perchloric acid and phosphoric acid；
First mixed solution is added in crystalline flake graphite, 20 DEG C ~ 45 DEG C are stirred to react 15min ~ 35min, and it is mixed to obtain first
Zoarium system；
Configure the second mixed solution, including potassium permanganate, perchloric acid；
Second mixed solution is added in first mixed system, 20 DEG C ~ 45 DEG C are stirred to react 5min ~ 15min, obtain
Second mixed system；
Second mixed system is filtered to take into solid, and washing to washing lotion is neutrality, obtains head product；
The head product is placed in 850 DEG C ~ 1000 DEG C environment calcination no longer to change to volume, obtains the expanded graphite；
Wherein, in the first mixed system preparation step, the crystalline flake graphite and first mixed solution
Ratio be (2 ~ 4) g:(1 ~ 8) mL；
In first mixed solution, the ratio of the sodium chlorate, the perchloric acid and the phosphoric acid be (0.1 ~ 2) g:(1 ~
6) mL:(0.1 ~ 2) mL；
Potassium permanganate described in second mixed solution, the perchloric acid ratio be (0.1 ~ 2) g:(1 ~ 6) mL；
The ratio of second mixed solution and first mixed solution is 3:4 ~ 6:5.
2. the preparation method of expanded graphite according to claim 1, which is characterized in that further include: described first is mixed
System carries out the step of first time ultrasonic vibration 5min ~ 10min, and ultrasonic power is 500w ~ 800w.
3. the preparation method of expanded graphite according to claim 1 or 2, which is characterized in that further include: described second is mixed
The step of zoarium system carries out second of ultrasonic vibration 5min ~ 10min, ultrasonic power are 1500w ~ 2000w.
4. the preparation method of expanded graphite according to claim 1, which is characterized in that the first mixed system preparation step
In rapid, the whipping step are as follows: 80r/min ~ 120r/min stirring 0 ~ 5min, 280r/min ~ 350r/min stirring 10min ~
30min；In the second mixed system preparation step, mixing speed are as follows: 280r/min ~ 350r/min.
5. the preparation method of expanded graphite according to claim 3, which is characterized in that after second of ultrasonic step
Further include the steps that decolourizing to the second hybrid system.
6. the preparation method of expanded graphite according to claim 5, which is characterized in that the decolorization process are as follows: described
The hydrogen peroxide that volume fraction is 10% ~ 40% is added in second mixed system, until second mixed system is colourless.
7. the preparation method of expanded graphite according to claim 1, which is characterized in that further include before the calcination step
The step of head product is dried, drying temperature are 40 DEG C ~ 65 DEG C, and drying time is 2h ~ 4h.
8. the preparation method of expanded graphite according to claim 1, which is characterized in that the washing lotion is water；The scale
Graphite mesh number is not more than 35 mesh.
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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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| 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 |
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Address after: Room 101-303, floor 3, building 4, courtyard 7, Yongze North Road, Haidian District, Beijing 100044 Patentee after: Beijing Dingchen Graphite Technology Co.,Ltd. Address before: 100044 courtyard 1, Yongze North Road, Yongfeng Industrial base, Haidian District, Beijing Patentee before: BEIJING DINGCHEN SUPERCONDUCTOR TECHNOLOGY Co.,Ltd. |