CN107500286A - Micro crystal graphite bulking process - Google Patents
Micro crystal graphite bulking process Download PDFInfo
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- CN107500286A CN107500286A CN201710915322.2A CN201710915322A CN107500286A CN 107500286 A CN107500286 A CN 107500286A CN 201710915322 A CN201710915322 A CN 201710915322A CN 107500286 A CN107500286 A CN 107500286A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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Abstract
The invention discloses micro crystal graphite bulking process, and it comprises the following steps：Step 1: micro crystal graphite raw mill is taken to the micro crystal graphite powder that granularity is 50 mesh；Step 2: after configuring intercalant solution according to mass ratio, the micro crystal graphite powder in step 1 is well mixed into intercalant solution；Step 3: oxidant is mixed into according to mass ratio, and the reaction time is more than 60min；Step 4: the mixed reactant after step 3 is filtered successively, rinsed, dried, then expanded acquisition expanded graphite, wherein, in step 4, during drying, water content is dried to as 8% 12% (wt), when expanded, carry out expanded using Muffle furnace and stops at 820 DEG C 950 DEG C 5s 10s；Natural micro crystal graphite is less than 1 μm in crystallite set and crystal particle diameter, only under an electron microscope just it is observed that its crystalline form, so the present invention selects suitable puffing time, swelling temperature and expanded moisture etc., the added value and scientific and technological content of microcrystalline graphite product are improved, 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 using micro crystal graphite as the expanded work of the micro crystal graphite of raw material
Skill.
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.
But in the prior art, the expanded raw material used of graphite is all natural flake graphite, especially big particle diameter squama
Piece graphite.
Therefore, a kind of micro crystal graphite bulking process using micro crystal graphite as raw material is now provided.
The content of the invention
Therefore, the present invention provides a kind of micro crystal graphite bulking process using micro crystal graphite as raw material.
Therefore, the invention provides micro crystal graphite bulking process, it comprises the following steps：
Step 1: micro crystal graphite raw mill is taken to the micro crystal graphite powder that granularity is 50 mesh；
Step 2: after configuring intercalant solution according to mass ratio, the micro crystal graphite powder in step 1 is well mixed to intercalation
In agent solution；
Step 3: oxidant is mixed into according to mass ratio, and the reaction time is more than 60min；
Step 4: filtered, rinsed, dried successively to the mixed reactant after step 3, then expanded acquisition expanded graphite；
Wherein, in step 4, during drying, it is 8%-12% (wt) to be dried to water content, when expanded, is carried out using Muffle furnace expanded
And stop 5s-10s at 820 DEG C -950 DEG C.
In step 1, micro crystal graphite that it is 98% for phosphorus content that micro crystal graphite raw material purifies before the milling is dried after grinding
Moisture, and it is standby to weigh 10g micro crystal graphite powders.
In step 2, intercalant solution is mixed by HCLO4, HNO3 and (CH3CO) 2O, and micro crystal graphite powder with
Intercalant solution is mixed by following mass ratio：C:HCLO4：HNO3:(CH3CO)2O=1:3.4:2:1.8, it is placed in magnetic agitation
It is well mixed in device under 40 DEG C of constant temperature.
In step 3, oxidant is set to CrO3, and micro crystal graphite powder is mixed with oxidant by following mass ratio：C:
CrO3=1:0.18。
In step 3, oxidant CrO3 is added in the mixed solution after step 2, be placed in reacting in 40 DEG C of constant temperature
90min。
In step 4, the PH that suction filtration backlash is washed till filtrate is 6-7, is subsequently placed into baking oven and dries 38-65min at 60 DEG C,
It is 8%-12% to water content.
When expanded, it is put into Muffle furnace and 6s progress expanding treatments, acquisition >=120ml/g expansion stone is stopped at 930 DEG C
Ink.
When expanded, it is put into Muffle furnace and 8s progress expanding treatments, acquisition >=115.3ml/g expansion is stopped at 850 DEG C
Graphite.
The present invention has the following advantages that part relative to prior art：
The micro crystal graphite bulking process of the present invention is specific to natural micro crystal graphite and set because natural micro crystal graphite with it is natural
Crystalline flake graphite is compared, and it is typically in crystallite aggregate, and the crystal particle diameter of natural micro crystal graphite is less than 1 μm, only in electron microscopic
Just it is observed that its crystalline form, so the present invention is directed to natural micro crystal graphite, passes through the intercalator from suitable micro crystal graphite under mirror
With oxidant, and selection suitable puffing time, swelling temperature and expanded moisture etc., the added value of microcrystalline graphite product is improved
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 expanded relevant parameter schematic diagram one of micro crystal graphite of the present invention；
Fig. 2 is the expanded relevant parameter schematic diagram two of micro crystal graphite of the present invention；
Fig. 3 is the expanded relevant parameter schematic diagram three of micro crystal graphite of the present invention；
Fig. 4 is the expanded relevant parameter schematic diagram four of micro crystal graphite of the present invention；
Fig. 5 is the expanded relevant parameter schematic diagram five of micro crystal graphite of the present invention；
Fig. 6 is the expanded relevant parameter schematic diagram six of micro crystal graphite of the present invention.
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 shown in Figure 1,2 and 3, micro crystal graphite bulking process 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 50 mesh；
Step 2: after configuring intercalant solution according to mass ratio, the micro crystal graphite powder in step 1 is well mixed to intercalation
In agent solution；
Step 3: oxidant is mixed into according to mass ratio, and the reaction time is more than 60min；
Step 4: filtered, rinsed, dried successively to the mixed reactant after step 3, then expanded acquisition expanded graphite；
Wherein, in step 4, during drying, it is 8%-12% (wt) to be dried to water content, when expanded, is carried out using Muffle furnace expanded
And stop 5s-10s at 820 DEG C -950 DEG C.
The micro crystal graphite bulking process of the present embodiment is specific to natural micro crystal graphite and set, because natural micro crystal graphite
Compared with natural flake graphite, it is typically in crystallite aggregate, and the crystal particle diameter of natural micro crystal graphite is less than 1 μm, only in electricity
Just it is observed that its crystalline form, so the present invention is directed to natural micro crystal graphite, is adapted to micro crystal graphite by selecting under sub- microscope
Intercalator and oxidant, and selection suitable puffing time, swelling temperature and expanded moisture etc., improve microcrystalline graphite product
Added value and scientific and technological content, while make the development prospect of micro crystal graphite industry broader.
Moisture exists in the form of being distributed in two kinds of expansible graphite surface and graphite layers in expansible graphite, but studies
Show, the moisture on expansible graphite surface is to the high temperature puffing of expansible graphite without contribution, and the moisture of graphite layers is in high temperature
Contribute to during gasification it is expanded, its show be not expansible graphite moisture it is the higher the better；If moisture is too high, due to
The moisture of graphite layers is substantially certain, so substantial amounts of attachment of moisture is in graphite surface, to expanded no contribution, while largely
Attachment of moisture on the surface of expansible graphite, in high temperature puffing, moisture evaporation can absorb substantial amounts of heat and cause true
The decline of swelling temperature, so as to reduce expansion ratio.
Specifically, in step 1, micro crystal graphite that it is 98% for phosphorus content that micro crystal graphite raw material purifies before the milling is ground
Moisture is dried after mill, and it is standby to weigh 10g micro crystal graphite powders.
In step 2, intercalant solution is mixed by HCLO4, HNO3 and (CH3CO) 2O, and micro crystal graphite powder with
Intercalant solution is mixed by following mass ratio：
C:HCLO4：HNO3:(CH3CO)2O=1:3.4:2:1.8, it is placed in magnetic stirring apparatus mixing under 40 DEG C of constant temperature
It is even.
In the present embodiment, intercalant solution is mixed by HCLO4, HNO3 and (CH3CO) 2O three, by microlite
Ink powder body is mixed evenly, and the mixing is carried out in magnetic stirring apparatus and under 40 DEG C of constant temperature, and meets C:HCLO4：
HNO3:(CH3CO)2O=1:3.4:2:1.8 mass ratio.
Further, in step 3, oxidant is set to CrO3, and micro crystal graphite powder is mixed with oxidant by following mass ratio
Close：C:CrO3=1:0.18；In the present embodiment, as shown in figure 1, in the case of other conditions all identical, C:CrO3 quality
Than from 1:0.02 gradually increase, then the expanded volume of micro crystal graphite constantly increases, and in C:CrO3 mass ratio not 1:0.18
When, the expanded volume of micro crystal graphite reaches maximum；Therefore in the present embodiment, preferably C:CrO3 mass ratio is 1:0.18.
In step 3, oxidant CrO3 is added in the mixed solution after step 2, be placed in reacting in 40 DEG C of constant temperature
90min.As shown in Fig. 2 in the case where other conditions are constant, when the reaction time is 90min, micro crystal graphite it is expanded
Volume reaches maximum, and the reaction time shortens or increase can all cause the expanded volume of micro crystal graphite relatively reduced, therefore this implementation
Example preferably reaction time is 90min；Meanwhile as shown in figure 3, in the case where other conditions are constant, reaction temperature is 40 DEG C
When, the expanded volume of micro crystal graphite is maximum, and reaction temperature can all cause the swollen of micro crystal graphite higher or lower than this temperature
Change volume relative decrease, therefore the present embodiment preferable reaction temperature is 40 DEG C.
On the basis of above-described embodiment, in step 4, the PH that suction filtration backlash is washed till filtrate is 6-7, is subsequently placed into baking oven
In dry 38-65min at 60 DEG C, be 8%-12% to water content.In the present embodiment, preferably PH is 6, is dried in 60 DEG C of baking oven
In dry 60min, the inflatable micro crystal graphite that water content is 9.86% is obtained, to realize the maximum expanded volume of micro crystal graphite.
Wherein, as shown in Fig. 4,5 and 6, as the preferred embodiment of the present embodiment, when expanded, it is put into Muffle furnace simultaneously
8s, which is stopped, at 850 DEG C carries out expanding treatment, acquisition >=115.3ml/g expanded graphite.
As disposable embodiment, if changing the expanded graphite that Condition for expansion will obtain different expanded volumes, such as：It is swollen
During change, it is put into Muffle furnace and 6s progress expanding treatments, acquisition >=120ml/g expanded graphite is stopped at 930 DEG C.
As described in Figure 4, in the case where other conditions are constant, when puffing time is 8s, the expanded volume of micro crystal graphite
Maximum, after the residence time is more than 8s, its expanded volume constantly reduces, and when the residence time is 2-8s, its expanded volume is continuous
Increase, and reach maximum expanded volume in 8s.
As shown in figure 5, in the case where other conditions are constant, when swelling temperature is 850 DEG C, the extruded body of micro crystal graphite
Product reaches maximum, all expanded volume will be caused to diminish more than or less than 850 DEG C.
As shown in fig. 6, in the case of other conditions are all constant, when the interlayer water content of micro crystal graphite is 9.86%, its is swollen
It is maximum to change volume, when water content is other percentage values, expanded volume all relative decreases of micro crystal graphite.
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 (8)
1. micro crystal graphite bulking process, 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 50 mesh；
Step 2: after configuring intercalant solution according to mass ratio, the micro crystal graphite powder in step 1 is well mixed to intercalation
In agent solution；
Step 3: oxidant is mixed into according to mass ratio, and the reaction time is more than 60min；
Step 4: filtered, rinsed, dried successively to the mixed reactant after step 3, then expanded acquisition expanded graphite；
Wherein, in step 4, during drying, it is 8%-12% (wt) to be dried to water content, when expanded, is carried out using Muffle furnace expanded
And stop 5s-10s at 820 DEG C -950 DEG C.
2. micro crystal graphite bulking process according to claim 1, it is characterised in that：In step 1, micro crystal graphite raw material is being ground
Purification is the micro crystal graphite that phosphorus content is 98% before mill, moisture is dried after grinding, and it is standby to weigh 10g micro crystal graphite powders.
3. micro crystal graphite bulking process according to claim 1, it is characterised in that：In step 2, intercalant solution by
HCLO4, HNO3 and (CH3CO) 2O are mixed, and micro crystal graphite powder is mixed with intercalant solution by following mass ratio：C:
HCLO4：HNO3:(CH3CO)2O=1:3.4:2:1.8, it is placed in magnetic stirring apparatus being well mixed under 40 DEG C of constant temperature.
4. micro crystal graphite bulking process according to claim 3, it is characterised in that：In step 3, oxidant is set to CrO3, and
Micro crystal graphite powder is mixed with oxidant by following mass ratio：C:CrO3=1:0.18.
5. micro crystal graphite bulking process according to claim 4, it is characterised in that：In step 3, oxidant CrO3 is added
In mixed solution after step 2, it is placed in reacting 90min in 40 DEG C of constant temperature.
6. micro crystal graphite bulking process according to claim 1, it is characterised in that：In step 4, filter backlash and be washed till filtrate
PH is 6-7, is subsequently placed into baking oven and dries 38-65min at 60 DEG C, is 8%-12% to water content.
7. micro crystal graphite bulking process according to claim 6, it is characterised in that：When expanded, it is put into Muffle furnace and at 930 DEG C
Stop 6s and carry out expanding treatment, acquisition >=120ml/g expanded graphite.
8. micro crystal graphite bulking process according to claim 6, it is characterised in that：When expanded, it is put into Muffle furnace and at 850 DEG C
Stop 8s and carry out expanding treatment, acquisition >=115.3ml/g expanded graphite.
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| CN201710915322.2A CN107500286A (en) | 2017-09-30 | 2017-09-30 | Micro crystal graphite bulking process |
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Citations (6)
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|---|---|---|---|---|
| CN1224693A (en) * | 1998-01-24 | 1999-08-04 | 北京华锐新材料技术发展有限公司 | Chemical graft process to prepare expansive graphite |
| CN1453209A (en) * | 2003-04-30 | 2003-11-05 | 中国科学院山西煤炭化学研究所 | Prepn of sulfur-free low-ash high-purity expanded graphite |
| CN101100298A (en) * | 2007-08-07 | 2008-01-09 | 哈尔滨工程大学 | Method for preparing expanded graphite |
| CN103881139A (en) * | 2014-03-10 | 2014-06-25 | 高碑店市顺新化工有限公司 | Multifunctional graphite interlayer compound as well as preparation method and application thereof |
| CN104157863A (en) * | 2014-08-22 | 2014-11-19 | 东莞市长安东阳光铝业研发有限公司 | Preparation method of micro-expansive graphite anode material |
| 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 CN201710915322.2A patent/CN107500286A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1224693A (en) * | 1998-01-24 | 1999-08-04 | 北京华锐新材料技术发展有限公司 | Chemical graft process to prepare expansive graphite |
| CN1453209A (en) * | 2003-04-30 | 2003-11-05 | 中国科学院山西煤炭化学研究所 | Prepn of sulfur-free low-ash high-purity expanded graphite |
| CN101100298A (en) * | 2007-08-07 | 2008-01-09 | 哈尔滨工程大学 | Method for preparing expanded graphite |
| CN103881139A (en) * | 2014-03-10 | 2014-06-25 | 高碑店市顺新化工有限公司 | Multifunctional graphite interlayer compound as well as preparation method and application thereof |
| CN104157863A (en) * | 2014-08-22 | 2014-11-19 | 东莞市长安东阳光铝业研发有限公司 | Preparation method of micro-expansive graphite anode material |
| CN104556022A (en) * | 2015-01-27 | 2015-04-29 | 西南科技大学 | Method for preparing expanded microcrystal graphite material from microcrystal graphite |
Non-Patent Citations (2)
| Title |
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| 李哲等: ""水分对可膨胀石墨膨胀容积的影响"", 《非金属矿》 * |
| 王太津等: "用CrO3作氧化剂制备无硫可膨胀石墨", 《广州化工》 * |
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Application publication date: 20171222 |