CN107572515A - The preparation method of inflatable micro crystal graphite - Google Patents
The preparation method of inflatable micro crystal graphite Download PDFInfo
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- CN107572515A CN107572515A CN201710915513.9A CN201710915513A CN107572515A CN 107572515 A CN107572515 A CN 107572515A CN 201710915513 A CN201710915513 A CN 201710915513A CN 107572515 A CN107572515 A CN 107572515A
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- micro crystal
- crystal graphite
- inflatable
- preparation
- intercalator
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Abstract
The invention discloses the preparation method of inflatable micro crystal graphite, and it includes：Step 1: micro crystal graphite raw mill is taken to the micro crystal graphite powder that granularity is 30 700 mesh；Step 2: the micro crystal graphite powder in step 1 is uniformly mixed with intercalator, strong oxidizer successively, inflatable micro crystal graphite acidic suspension is obtained；Inflatable micro crystal graphite is obtained after processing Step 3: to the inflatable micro crystal graphite acidic suspension obtained in step 2 be filtered, washed and dried；Wherein, the intercalator is set to the concentrated sulfuric acid, and the oxidant is set to potassium permanganate and hydrogen peroxide；The inflatable micro crystal graphite obtained after expanded processing has more excellent electrical property, this use for battery and electrode material for super capacitor etc. is very important, the added value and scientific and technological content of microcrystalline graphite product are improved, while makes the development prospect of micro crystal graphite industry broader.
Description
Technical field
The present invention relates to graphite expansion field, more particularly to a kind of inflatable micro crystal graphite using micro crystal graphite as raw material
Preparation method.
Background technology
Graphite crystal has the galvanized hexagonal wire mesh plane layer structure that is made up of carbon, and the carbon atom on layer plane is with strong
Covalent bonding together, and layer is combined with interlayer with Van der Waals force, and with reference to very weak, and interfloor distance is larger.Therefore, appropriate
Under conditions of, a variety of chemical substances such as acid, alkali metal, salt can be inserted into graphite layers, and combine to form new change with carbon atom
Learn phase --- compound between graphite layers (Graphite Intercalation on Compounds, abbreviation GIC)；This interlayer
Compound can be decomposed rapidly moment when being heated to proper temperature, is produced a large amount of gases, graphite is axially expanded into worm
The novel substance of shape, i.e. expanded graphite, and this unexpanded compound between graphite layers are exactly expansible graphite.
Micro crystal graphite compares with Scaly graphite, and crystal habit has prominent otherness, and the former is in inlay aggregate,
Small, the visible morphon under electron microscope of grain；The latter disperses flakey in monocrystalline, and chip naked eyes are visible.The two is in chemistry
Reactive nature, crystalline orientation etc. have notable difference.Scaly graphite scale is big, aggregate favorable orientation；But in electricity
, it is necessary to which the good graphite material of poor orientation, homogenieity, is often carried out Scaly graphite for this in pond and electrode material for super capacitor
Spheroidization processing, but result is unsatisfactory；And micro crystal graphite particle is tiny, aggregate poor orientation, homogenieity are good, expanded place
The inflatable micro crystal graphite obtained after reason has more excellent electrical property, and this is for battery and electrode material for super capacitor etc.
Use be very important.
Therefore, a kind of preparation method using micro crystal graphite as the inflatable micro crystal graphite of raw material is now provided.
The content of the invention
Therefore, the present invention provides a kind of preparation method using micro crystal graphite as the inflatable micro crystal graphite of raw material.
The preparation method of the inflatable micro crystal graphite of the present invention, it comprises the following steps：
Step 1: micro crystal graphite raw mill is taken to the micro crystal graphite powder that granularity is 30-700 mesh；
Step 2: the micro crystal graphite powder in step 1 is uniformly mixed with intercalator, strong oxidizer successively, obtaining can be swollen
Swollen micro crystal graphite acidic suspension；
Step 3: the inflatable micro crystal graphite acidic suspension obtained in step 2 is carried out being filtered, washed and dried place
Inflatable micro crystal graphite is obtained after reason；
Wherein, the intercalator is set to the concentrated sulfuric acid, and the oxidant is set to potassium permanganate and hydrogen peroxide.
In step 1, micro crystal graphite that it is 99% for phosphorus content that micro crystal graphite raw material purifies before the milling.
In step 2, micro crystal graphite powder and intercalator are mixed in following ratio：Micro crystal graphite powder (g): intercalator
(ml)=5: 1, carry out in a kettle and stirring reaction 3-5min obtains both mixtures.
In step 2, mixture mixes with hydrogen peroxide again after being mixed with potassium permanganate.
Mixture is mixed with potassium permanganate by following mass ratio：Micro crystal graphite powder: potassium permanganate=1: 0.05, and in room
Stirred under temperature.
Mixture is mixed with hydrogen peroxide by following mass ratio：Micro crystal graphite powder: hydrogen peroxide=1: 0.2, and at 40 DEG C
Stirring reaction 2.0h.
In step 3, during filtering, the maximum diameter of hole of filter membrane is 0.5~20 μm, during washing, using deionized water by filter residue
Wash to the filtrate that PH is 5-7.
When drying, dewater treatment is carried out first, then carries out drying and processing again.
Dried using dryer, it dries 8h-13h at 50-70 DEG C, obtains the inflatable of the coefficient of expansion >=150
Micro crystal graphite.
The present invention has the following advantages that part relative to prior art：
The preparation method of the inflatable micro crystal graphite of the present invention is specific to micro crystal graphite setting, and micro crystal graphite particle is thin
Small, aggregate poor orientation, homogenieity are good, and the inflatable micro crystal graphite obtained after expanded processing has more excellent electrical
Can, this use for battery and electrode material for super capacitor etc. is very important, improves the additional of microcrystalline graphite product
Value and scientific and technological content, while make the development prospect of micro crystal graphite industry broader.
Brief description of the drawings
, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical scheme of the prior art
The required accompanying drawing used is briefly described in embodiment or description of the prior art, it should be apparent that, in describing below
Accompanying drawing is some embodiments of the present invention, for those of ordinary skill in the art, before creative work is not paid
Put, other accompanying drawings can also be obtained according to these accompanying drawings.
Fig. 1 is the micro crystal graphite raw material of the present invention and the X-ray diffractogram of inflatable micro crystal graphite；
Fig. 2, which is that the inflatable micro crystal graphite obtained by the preparation of the present invention is high, matches somebody with somebody scanning electron microscopy picture.
Embodiment
Technical scheme is clearly and completely described below in conjunction with accompanying drawing, it is clear that described implementation
Example is part of the embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, ordinary skill
The every other embodiment that personnel are obtained under the premise of creative work is not made, belongs to the scope of protection of the invention.
As long as in addition, technical characteristic involved in invention described below different embodiments non-structure each other
It is be combined with each other into conflict can.
As illustrated in fig. 1 and 2, the preparation method of inflatable micro crystal graphite is present embodiments provided, it comprises the following steps：
Step 1: micro crystal graphite raw mill is taken to the micro crystal graphite powder that granularity is 30-700 mesh；
Step 2: the micro crystal graphite powder in step 1 is uniformly mixed with intercalator, strong oxidizer successively, obtaining can be swollen
Swollen micro crystal graphite acidic suspension；
Step 3: the inflatable micro crystal graphite acidic suspension obtained in step 2 is carried out being filtered, washed and dried place
Inflatable micro crystal graphite is obtained after reason；
Wherein, the intercalator is set to the concentrated sulfuric acid, and the oxidant is set to potassium permanganate and hydrogen peroxide.
The preparation method of the inflatable micro crystal graphite of the present embodiment is specific to micro crystal graphite setting, micro crystal graphite particle
Tiny, aggregate poor orientation, homogenieity are good, and the inflatable micro crystal graphite obtained after expanded processing has more excellent electricity
Performance, this use for battery and electrode material for super capacitor etc. is very important, improves the attached of microcrystalline graphite product
Value added and scientific and technological content, while make the development prospect of micro crystal graphite industry broader.
As preferred embodiment, in step 1, it is 99% that micro crystal graphite raw material purifies as phosphorus content before the milling
Micro crystal graphite.
Specifically, in step 2, micro crystal graphite powder and intercalator are mixed in following ratio：Micro crystal graphite powder (g):
Intercalator (ml)=5: 1, carry out in a kettle and stirring reaction 3-5min obtains both mixtures.In the present embodiment,
Micro crystal graphite powder and intercalator are stirred in a kettle with the ratio of the corresponding 1 milliliter of intercalator of every 5 grams of micro crystal graphite powders
Uniformly and react 3 minutes to 5 minutes, so that micro crystal graphite and intercalator hybrid reaction are uniform.
In step 2, mixture mixes with hydrogen peroxide again after being mixed with potassium permanganate.
Specifically, mixture is mixed with potassium permanganate by following mass ratio：Micro crystal graphite powder: potassium permanganate=1:
0.05, and be stirred at room temperature uniformly；Mixture is mixed with hydrogen peroxide by following mass ratio：Micro crystal graphite powder: hydrogen peroxide=1
: 0.2, and the stirring reaction 2.0h at 40 DEG C.
In step 3, during filtering, the maximum diameter of hole of filter membrane is 0.5~20 μm, during washing, using deionized water by filter residue
Wash to the filtrate that PH is 5-7.
When drying, dewater treatment is carried out first, then carries out drying and processing again.
Dried using dryer, it dries 8h-13h at 50-70 DEG C, obtains the inflatable of the coefficient of expansion >=150
Micro crystal graphite.
It is as follows as the specific embodiment of the present invention, its concrete condition：
First, choose the micro crystal graphite that phosphorus content is 99% and be ground to the micro crystal graphite powder that granularity is 500 mesh, then
100g micro crystal graphite powders accurately are weighed, are put into reactor；Then, concentrated sulfuric acid valve is opened according to micro crystal graphite powder (g): is inserted
The ratio of layer agent (ml)=5: 1 injects the concentrated sulfuric acid (98%) into reactor, and opens air-flow and mechanical agitation, makes the two reaction
Reach full and uniform mixing within 20 minutes；5g potassium permanganate is then added in the case where not stopping stirring and is reacted 5 minutes, has been reacted
Into rear 20 milliliters of hydrogen peroxide of injection (content is less than 20%) and react two hours, be fully after completion of the reaction transferred to above-mentioned material
Washing to PH values are not less than 5 in scrubbing tower, then place into and dewater treatment is carried out in dewaterer, and 60 DEG C are sent into after dehydration
Dried in dryer, finally obtain the inflatable micro crystal graphite that the coefficient of expansion is 230.
Obviously, above-described embodiment is only intended to clearly illustrate example, and is not the restriction to embodiment.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 change or
Change.There is no necessity and possibility to exhaust all the enbodiments.And the obvious change thus extended out or
Among changing still in the protection domain of the invention.
Claims (9)
1. the preparation method of inflatable micro crystal graphite, it is characterised in that：It comprises the following steps：
Step 1: micro crystal graphite raw mill is taken to the micro crystal graphite powder that granularity is 30-700 mesh；
Step 2: the micro crystal graphite powder in step 1 is uniformly mixed with intercalator, strong oxidizer successively, obtain inflatable micro-
Spar ink acidic suspension；
Step 3: the inflatable micro crystal graphite acidic suspension obtained in step 2 is carried out after being filtered, washed and dried processing
Obtain inflatable micro crystal graphite；
Wherein, the intercalator is set to the concentrated sulfuric acid, and the oxidant is set to potassium permanganate and hydrogen peroxide.
2. the preparation method of inflatable micro crystal graphite according to claim 1, it is characterised in that：In step 1, micro crystal graphite
The micro crystal graphite that it is 99% for phosphorus content that raw material purifies before the milling.
3. the preparation method of inflatable micro crystal graphite according to claim 1, it is characterised in that：In step 2, micro crystal graphite
Powder and intercalator are mixed in following ratio：Micro crystal graphite powder（g）：Intercalator（ml）=5:1, carry out and stir in a kettle
Mix reaction 3-5min and obtain both mixtures.
4. the preparation method of inflatable micro crystal graphite according to claim 3, it is characterised in that：In step 2, mixture with
Mixed again with hydrogen peroxide after potassium permanganate mixing.
5. the preparation method of inflatable micro crystal graphite according to claim 4, it is characterised in that：Mixture is with potassium permanganate by such as
Lower mass ratio mixing：Micro crystal graphite powder：Potassium permanganate=1：0.05, and be stirred at room temperature uniformly.
6. the preparation method of inflatable micro crystal graphite according to claim 5, it is characterised in that：Mixture is with hydrogen peroxide by as follows
Mass ratio mixes：Micro crystal graphite powder：Hydrogen peroxide=1：0.2, and the stirring reaction 2.0h at 40 DEG C.
7. the preparation method of inflatable micro crystal graphite according to claim 1, it is characterised in that：In step 3, during filtering, filter
The maximum diameter of hole of film is 0.5~20 μm, during washing, uses filtrate of the deionized water by residue washing to PH for 5-7.
8. the preparation method of inflatable micro crystal graphite according to claim 7, it is characterised in that：When drying, it is dehydrated first
Processing, then carries out drying and processing again.
9. the preparation method of inflatable micro crystal graphite according to claim 8, it is characterised in that：Dried using dryer,
It dries 8h-13h at 50-70 DEG C, obtains the inflatable micro crystal graphite of the coefficient of expansion >=150.
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| CN201710915513.9A CN107572515A (en) | 2017-09-30 | 2017-09-30 | The preparation method of inflatable micro crystal graphite |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101100298A (en) * | 2007-08-07 | 2008-01-09 | 哈尔滨工程大学 | Method for preparing expanded graphite |
| CN104445169A (en) * | 2014-12-03 | 2015-03-25 | 安徽百特新材料科技有限公司 | Method for preparing grapheme by means of aqueous phase cutting and stripping |
| CN104556022A (en) * | 2015-01-27 | 2015-04-29 | 西南科技大学 | Method for preparing expanded microcrystal graphite material from microcrystal graphite |
-
2017
- 2017-09-30 CN CN201710915513.9A patent/CN107572515A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101100298A (en) * | 2007-08-07 | 2008-01-09 | 哈尔滨工程大学 | Method for preparing expanded graphite |
| CN104445169A (en) * | 2014-12-03 | 2015-03-25 | 安徽百特新材料科技有限公司 | Method for preparing grapheme by means of aqueous phase cutting and stripping |
| CN104556022A (en) * | 2015-01-27 | 2015-04-29 | 西南科技大学 | Method for preparing expanded microcrystal graphite material from microcrystal graphite |
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