CN106629703A - Method for preparing highly-expandable low-sulfur graphite intercalation compound - Google Patents
Method for preparing highly-expandable low-sulfur graphite intercalation compound Download PDFInfo
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Abstract
The invention provides a method for preparing a highly-expandable low-sulfur graphite intercalation compound and relates to the technical field of graphite. The method includes heating natural flake graphite in water bath; adding an intercalator to soak the natural flake graphite; adding an oxidizing agent, and reacting so as to obtain a reaction product; subjecting the reaction product to water scrubbing, filtering the scrubbed reaction product, and drying the filtered reaction product so as to obtain acidized graphite; heating the acidized graphite in water bath; adding perchloric acid and acetic acid to soak the acidized graphite; adding an oxidizing agent to react so as to obtain a product; subjecting the product to water scrubbing, filtering the scrubbed product and drying the filtered product. The method has the advantages that no sulfur element is introduced into a preparation process of the expandable low-sulfur graphite intercalation compound, so that the sulfur content in expandable graphite is decreased, and the highly-expandable low-sulfur graphite intercalation compound is excellent in expandability.
Description
Technical field
The present invention relates to graphite technology field, is related to a kind of preparation side of high expansiveness low-sulfur graphite intercalation compound
Method.
Background technology
Expanded graphite is the loose porous particle of vermiform of the network-like hole series structure for having abundant.Its surface activity height,
Bulk density is little, thermal conductivity is adjustable, adsorptivity is strong, chemical stability is good, nontoxic, pollution-free, can make flexible foils, every
Hot body, conducting polymer, electrode, adsorbent etc., are widely studied and application.
Expanded graphite is obtained by graphite intercalation compound (GIC) high-temperature expansion, as the precursor of expanded graphite,
The chemical composition and performance of GIC has a major impact to final expanded product expanded graphite, and the composition of GIC and performance are depended on
It adopts which kind of preparation method and technique.Prepare GIC and be most commonly used that direct chemical oxidization method, will native graphite and oxidant
Mix by certain amount ratio with intercalator, at moderate temperatures stirring reaction certain hour, after being then washed to neutrality and drying
Obtain GIC.At present, the research for preparing GIC with regard to direct chemical oxidization method is concentrated mainly on the lifting of GIC expansion effects, sulfur and contains
The aspects such as the reduction of the reduction of amount, the reduction of expansion temperature, energy consumption and cost.
Because direct chemical oxidization method tends not to give full play to the effect that oxidant reacts graphite intercalation, it is unfavorable for carrying
Rise expansion effect, reduce expansion temperature and energy consumption and cost.In order to further improve the intercalation effect of GIC, Han Zhidong etc. new
Type material with carbon element, to report on 2009,24 (4) and obtain nitric acid/nitrate/sulphuric acid ternary intercalation GIC using substep graft process；Jiang Shuxing
Deng in non-ore deposit metal, report on 2013,36 (6) with potassium permanganate as oxidant, respectively with 36% acetic acid+concentrated sulphuric acid as once
Intercalator, concentrated nitric acid+concentrated sulphuric acid are the method that secondary intercalation agent prepares GIC；Zhang Dawei etc. in Chemical Engineer, 2013,137
(2) method that the GIC of sulphuric acid intercalation is further carried out into secondary intercalation with phosphorus-containing compound is reported on.
Although the substep graft process in above-mentioned report can improve the intercalation effect of GIC, it adopts sulphuric acid for intercalator,
What is obtained is the graphite intercalation compound of sulfur-bearing, and the sulfur-containing compound for being unfavorable for environmental protection can be discharged during its expanded by heating,
And a certain amount of element sulphur can be also remained in gained expanded graphite, it is unfavorable for preparing low-sulphur expanded graphite.In order to ensure that height can be swollen
Swollen property and low sulfur content, Zhao Jijin etc. are reported with potassium permanganate as oxidant in optical precision engineering on 2014,22 (5), first
Afterwards the method that secondary intercalation prepares GIC is carried out as intercalator with nitric acid+phosphoric acid, nitric acid+acetic acid, the method can significantly reduce GIC
Sulfur content, but inflatable volume is up to 450ml/g, and expansion effect is not satisfactory.
The content of the invention
Not enough for prior art, the present invention provides a kind of preparation side of high expansiveness low-sulfur graphite intercalation compound
Method, solves the technical problem that graphite intercalation compound expansion effect is undesirable, sulfur content is high in prior art.
To realize object above, the present invention is achieved by the following technical programs：
A kind of preparation method of high expansiveness low-sulfur graphite intercalation compound, comprises the following steps：
S1, by natural flake graphite add flask in, heating in water bath, keeping temperature be 20 DEG C～30 DEG C；
S2, by intercalator add step S1 flask in, soak 3～7min of natural flake graphite, add oxidant, stir
30～50min is mixed, product is obtained, wherein the quality of natural flake graphite and the volume ratio of intercalator are 1：3～1：9, day
So crystalline flake graphite and the mass ratio of oxidant are 1：0.05～1：0.35；
S3, the product that step S2 is obtained is washed to into neutrality, is filtered, 30～50 DEG C of vacuum drying obtain being acidified stone
Ink；
S4, the acidifying graphite that step S3 is obtained is inserted in flask, heating in water bath, keeping temperature is 20 DEG C～30 DEG C；
S5, perchloric acid and acetic acid are separately added in the flask of step S3, are stirred, soak 3～7min of acidifying graphite,
Oxidant is added, 30～50min of stirring reaction obtains product, and the wherein quality of acidifying graphite is with the volume ratio of perchloric acid
1:1～1:4, the quality of acidifying graphite is 1 with the volume ratio of acetic acid:2～1:8, acidifying graphite is 1 with the mass ratio of oxidant:
0.05～1:0.2；
S6, the product that step S5 is obtained is washed to into neutrality, is filtered, 30～50 DEG C of vacuum drying, you can finally produced
Thing.
Preferably, step S2 and oxidant described in step S5 are in potassium permanganate, potassium dichromate, concentrated nitric acid, perchloric acid
It is a kind of.
Preferably, intercalator described in step S2 is concentrated nitric acid or perchloric acid.
Preferably, the concentration of the perchloric acid is 70%～72%.
Preferably, the acetic acid concentration is 99.5%.
Preferably, the quality of natural flake graphite described in step S2 and the volume ratio of intercalator are 1：6～1：7.
Preferably, natural flake graphite described in step S2 and the mass ratio of oxidant are 1：0.2～1：0.35.
Preferably, the quality of acidifying graphite described in step S5 and the volume ratio of perchloric acid are 1：1～1：3.
Preferably, the quality of acidifying graphite described in step S5 and the volume ratio of acetic acid are 1：4～1：5.
Preferably, acidifying graphite described in step S5 and the mass ratio of oxidant are 1：0.2.
The present invention provides a kind of preparation method of high expansiveness low-sulfur graphite intercalation compound, excellent compared with prior art
Put and be：
The present invention by using the efficiently oxidant without sulfur and intercalator, make to prepare the whole oxidation intercalation process of GIC without
Element sulphur is introduced, and had both avoided and the sulfur-containing compound for being unfavorable for environmental protection is discharged during GIC expanded by heating, is significantly reduced
Sulfur content in expanded product expanded graphite；
The high expansiveness low-sulfur graphite intercalation compound of the present invention has excellent expansiveness energy, can be seen by table 1
Go out, at 200 DEG C, inflatable volume has reached 380ml/g, and at 800 DEG C 600ml/g can be reached.This is swollen further to prepare
The expanded graphite that swollen rate is high, adsorptivity is strong, electromagnetic wave attenuation performance is excellent has established good material base.
The expansion character test result of the high expansiveness low-sulfur graphite intercalation compound of the invention of table 1
Description of the drawings
Fig. 1 is the expansion characteristics test chart of graphite intercalation compound prepared by the present invention；
Fig. 2 is the infrared spectrogram of graphite intercalation compound prepared by the present invention；
Fig. 3 is the X-ray diffraction spectrogram of graphite intercalation compound prepared by the present invention.
Specific embodiment
To make purpose, technical scheme and the advantage of the embodiment of the present invention clearer, with reference to embodiment to the present invention
Technical scheme in embodiment is clearly and completely described, it is clear that described embodiment is that a part of the invention is implemented
Example, rather than the embodiment of whole.Based on the embodiment in the present invention, those of ordinary skill in the art are not making creativeness
The every other embodiment obtained under the premise of work, belongs to the scope of protection of the invention.
In the examples below, using the type Fourier transform infrared spectroscopies of Nicolet 8700 of Nicolet companies of the U.S.
The infrared spectrum of the graphite intercalation compound of the instrument test present invention；Using the XRD-7000 type X-rays of Japanese SHIMADZU companies
Diffractometer tests its X-ray diffraction spectrum.
The expansiveness energy of graphite intercalation compound is characterized using swelling volume (Expanding volume, EV), it refers to
The graphite intercalation compound of unit mass expand at a certain temperature after volume, unit is ml/g.Its testing procedure is as follows：
(1) graphite intercalation compound that quality is m is weighed, 0.0001g is accurate to；(2) it is quickly loaded in the horse of design temperature
Not preheat in stove in the quartz beaker of 5min, and put back to immediately in stove；(3) quartz beaker is taken out after about 30 seconds, treats swollen in beaker
Proceeded in graduated cylinder after swollen product cooling, read its volume V and (read top surface highs and lows correspondence scale respectively, take
Both meansigma methodss).Then inflatable volume EV is calculated by formula (1).
EV=V/m (1)
Embodiment 1：
The preparation method of the high expansiveness low-sulfur graphite intercalation compound of the present embodiment, comprises the following steps：
S1, a certain amount of natural flake graphite being weighed as required, natural flake graphite being added in flask, water-bath adds
Heat, keeping temperature is 25 DEG C；
The mass volume ratio of S2, the natural flake graphite raw material specified according to table 2 and intercalator, measures the height of respective volume
Chloric acid, perchloric acid is added in the flask of step S1, natural flake graphite 5min is soaked, according still further to the natural scale that table 2 is specified
Graphite and the mass ratio of oxidant, weigh the potassium permanganate of respective quality, in being added to above-mentioned flask, stir 40min, obtain anti-
Answer product；
S3, the product that step S2 is obtained is washed to into neutrality, is filtered, 40 DEG C of vacuum drying obtain acidifying graphite；
S4, a certain amount of step S3 is weighed as required obtain acidifying graphite and insert in flask, heating in water bath, keeping temperature
For 25 DEG C；
The mass volume ratio of S5, the acidifying graphite specified according to table 2 and acetic acid, acidifying graphite and perchloric acid, measures respectively
The acetic acid of respective volume and perchloric acid are added in the flask of step S3, are stirred, and acidifying graphite 5min are soaked, according still further to table 2
The acidifying graphite specified and the mass ratio of potassium permanganate, weigh the potassium permanganate addition of respective quality, and stirring reaction 40min is obtained
To product；
S6, the product that step S5 is obtained is washed to into neutrality, is filtered, 40 DEG C of vacuum drying, you can obtain high expansiveness
Low-sulfur graphite intercalation compound.
Inflatable volume EV of the graphite intercalation compound under different expansion temperatures obtained in test the present embodiment, test knot
Fruit is respectively such as table 2.
Embodiment 2：
The preparation method of the high expansiveness low-sulfur graphite intercalation compound of the present embodiment, comprises the following steps：
S1, a certain amount of natural flake graphite being weighed as required, natural flake graphite being added in flask, water-bath adds
Heat, keeping temperature is 20 DEG C；
The mass volume ratio of S2, the natural flake graphite raw material specified according to table 2 and intercalator, measures the dense of respective volume
Nitric acid, concentrated nitric acid is added in the flask of step S1, natural flake graphite 3min is soaked, according still further to the natural scale that table 2 is specified
Graphite and the mass ratio of oxidant, weigh the potassium dichromate of respective quality, in being added to above-mentioned flask, stir 30min, obtain anti-
Answer product；
S3, the product that step S2 is obtained is washed to into neutrality, is filtered, 30 DEG C of vacuum drying obtain acidifying graphite；
S4, a certain amount of step S3 is weighed as required obtain acidifying graphite and insert in flask, heating in water bath, keeping temperature
For 20 DEG C；
The mass volume ratio of S5, the acidifying graphite specified according to table 2 and acetic acid, acidifying graphite and perchloric acid, measures respectively
The concentration of respective volume is that 99.5% acetic acid and concentration are in the flask that 70% perchloric acid adds step S3, and stirring is equal
It is even, acidifying graphite 3min is soaked, the acidifying graphite specified according still further to table 2 and the mass ratio of oxidant weigh the weight of respective quality
Neutral potassium chromate is added, and stirring reaction 30min obtains product；
S6, the product that step S5 is obtained is washed to into neutrality, is filtered, 30 DEG C of vacuum drying, you can obtain high expansiveness
Low-sulfur graphite intercalation compound.
Inflatable volume EV of the graphite intercalation compound under different expansion temperatures obtained in test the present embodiment, test knot
Fruit is respectively such as table 2.
Embodiment 3：
The preparation method of the high expansiveness low-sulfur graphite intercalation compound of the present embodiment, comprises the following steps：
S1, a certain amount of natural flake graphite being weighed as required, natural flake graphite being added in flask, water-bath adds
Heat, keeping temperature is 30 DEG C；
The mass volume ratio of S2, the natural flake graphite raw material specified according to table 2 and intercalator, measures the dense of respective volume
Nitric acid, concentrated nitric acid is added in the flask of step S1, natural flake graphite 7min is soaked, according still further to the natural scale that table 2 is specified
Graphite and the mass ratio of oxidant, weigh the perchloric acid of respective quality, in being added to above-mentioned flask, stir 50min, are reacted
Product；
S3, the product that step S2 is obtained is washed to into neutrality, is filtered, 50 DEG C of vacuum drying obtain acidifying graphite；
S4, a certain amount of step S3 is weighed as required obtain acidifying graphite and insert in flask, heating in water bath, keeping temperature
For 30 DEG C；
The mass volume ratio of S5, the acidifying graphite specified according to table 2 and acetic acid, acidifying graphite and perchloric acid, measures respectively
The concentration of respective volume is that 99.5% acetic acid and concentration are in the flask that 72% perchloric acid adds step S3, and stirring is equal
It is even, acidifying graphite 7min is soaked, the acidifying graphite specified according still further to table 2 and the mass ratio of oxidant weigh the weight of respective quality
Neutral potassium chromate is added, and stirring reaction 50min obtains product；
S6, the product that step S5 is obtained is washed to into neutrality, is filtered, 50 DEG C of vacuum drying, you can obtain high expansiveness
Low-sulfur graphite intercalation compound.
Inflatable volume EV of the graphite intercalation compound under different expansion temperatures obtained in test the present embodiment, test knot
Fruit is respectively such as table 2.
Embodiment 4：
Raw materials used same embodiment 1 in the preparation process of the high expansiveness low-sulfur graphite intercalation compound of the present embodiment, presses
Table 2 specifies raw material, oxidant, the amount ratio of intercalator of embodiment 4, repeats the operation of embodiment 1.Additionally, testing this enforcement
Acidifying graphite obtained in example step S3 and the step of S6 expandable bodies of the graphite intercalation compound under different expansion temperatures are obtained
Product EV, X-ray diffraction analysis, infrared spectrum analysiss, test result is shown in respectively Fig. 1, table 2, Fig. 2 and Fig. 3.
Figure it is seen that acidifying graphite is in 1112.7cm obtained in step S3-1、1087.6cm-1There is ClO in place4 -'s
Strong characteristic absorption peak, shows intercalator HClO4Graphite flake layer has been inserted；In 3429.7cm-1And 1631.4cm-1The strong absworption peak at place
It is H2The characteristic absorption peak of O, the micro-moisture in being attributable to sample and tabletting KBr.Graphite intercalation chemical combination obtained in step S6
Thing is in 1120.4cm-1、1089.5cm-1There is ClO in place4 -Characteristic absorption peak strengthened, illustrate at further intercalation
Reason improves intercalation efficiency；In 1770.3cm-1Place occurs in that the strong characteristic absorption peak of-COOH, illustrates through further intercalation
Process, CH3COOH has inserted graphite flake layer, equally in 3424.9cm-1And 1636.3cm-1The strong absworption peak at place be attributable to sample and
The tabletting micro-moisture of KBr.Because being not introduced into sulphuric acid during whole intercalation, the characteristic absorption related to sulfur is there are no
The appearance at peak.It is possible thereby to judge, intercalator HClO4、CH3COOH has inserted graphite flake layer, forms the graphite intercalation of low-sulfur
Compound.
Fig. 3 shows, for crystalline flake graphite, acidifying graphite obtained in step S3 and the step of S6 be obtained graphite intercalation
There is significant change the width of compound diffraction maximum and position, its spy at 2 θ=26.52 ° of correspondence graphite [002] crystal face
Levy peak to broaden and to low angle skew, the weak characteristic peak at 2 θ=55 ° of correspondence graphite [211] crystal face splits into weaker wider
New diffraction maximum.When EV is 600ml/g, 2 θ are reduced to 23.96 ° by 26.52 °, and the weak characteristic peak at 2 θ=55 ° has divided
Into four faint small peaks.Because intercalator HClO4And CH3COOH insertions graphite layers make it push open along C direction of principal axis, cause interlayer
Away from increase, i.e. d00lIncrease.According to Bragg equations, graphite layers away from increase, the corresponding angle of diffraction of diffraction maximum will be caused to reduce,
The diffraction maximum for having [00l] face is moved to low angle, and this shows the preparation method of the present invention, the cladding of graphite on C direction of principal axis
It is repeated cyclically arrangement architecture to be destroyed, intercalator preferably enters the interlayer of native graphite.
Embodiment 5：
Raw materials used same embodiment 1 in the preparation process of the high expansiveness low-sulfur graphite intercalation compound of the present embodiment, presses
Table 2 specifies raw material, oxidant, the amount ratio of intercalator of embodiment 5, repeats the operation of embodiment 1.
Inflatable volume EV of the graphite intercalation compound under different expansion temperatures obtained in test the present embodiment, test knot
Fruit is respectively such as table 2.
Embodiment 6：
Raw materials used same embodiment 1 in the preparation process of the high expansiveness low-sulfur graphite intercalation compound of the present embodiment, presses
Table 2 specifies raw material, oxidant, the amount ratio of intercalator of embodiment 6, repeats the operation of embodiment 1.
Inflatable volume EV of the graphite intercalation compound under different expansion temperatures obtained in test the present embodiment, test knot
Fruit is respectively such as table 2.
Comparative example 1：
Raw material, oxidant, the amount ratio of intercalator specified by table 2, repeats the operational approach of embodiment 1, this comparative example
In the preparation process of graphite intercalation compound, the intercalator of step S2 is pressed from the nitric acid of concentration 65% and the phosphoric acid of concentration 85%
According to 1:The mixed acid of 4 volume ratio composition, other raw materials are with embodiment 1.
Test inflatable volume EV of the graphite intercalation compound obtained in this comparative example under different expansion temperatures, test knot
Fruit is respectively such as table 2.
Comparative example 2：
By the amount ratio of the raw material, oxidant, intercalator specified in table 2, repeat the operational approach of embodiment 1, this contrast
In the preparation process of example graphite intercalation compound, perchloric acid changes the nitric acid that concentration is 65% in step S5, tests this comparative example
Inflatable volume EV of the obtained graphite intercalation compound under different expansion temperatures, test result is respectively such as table 2.
Graphite intercalation compound is inflatable under different expansion temperatures by obtained in table 2 and Fig. 1 can be seen that comparative example
Volume EV only up to reach 450ml/g, and the obtained graphite intercalation compound of the present invention under different expansion temperatures can be swollen
Swollen volume EV is in more than 550ml/g, it might even be possible to reach 600ml/g, and expansion character is significantly larger than comparative example, and this is further
Prepare the expanded graphite that dilatancy is high, adsorptivity is strong, electromagnetic wave attenuation is excellent and establish good material base.
The inflatable volume of oxidant, intercalator and its amount ratio and product GIC in the embodiments of the invention of table 2
In sum, the present invention is by using the efficiently oxidant without sulfur and intercalator, inserting the whole oxidation for preparing GIC
Layer process is introduced without element sulphur, had both avoided and the sulfur-containing compound for being unfavorable for environmental protection is discharged during GIC expanded by heating, is also shown
Work reduces the sulfur content in expanded product expanded graphite；
The high expansiveness low-sulfur graphite intercalation compound of the present invention has excellent expansion character, can be swollen at 200 DEG C
Swollen volume has reached 380ml/g, and at 800 DEG C 600ml/g can be reached, and is further to prepare that dilatancy is high, adsorptivity is strong, electricity
The excellent expanded graphite of magnetic wave Decay Rate has established good material base.
Above example only to illustrate technical scheme, rather than a limitation；Although with reference to the foregoing embodiments
The present invention has been described in detail, it will be understood by those within the art that：It still can be to aforementioned each enforcement
Technical scheme described in example is modified, or carries out equivalent to which part technical characteristic；And these modification or
Replace, do not make the spirit and scope of the essence disengaging various embodiments of the present invention technical scheme of appropriate technical solution.
Claims (10)
1. a kind of preparation method of high expansiveness low-sulfur graphite intercalation compound, it is characterised in that comprise the following steps：
S1, by natural flake graphite add flask in, heating in water bath, keeping temperature be 20 DEG C～30 DEG C；
S2, intercalator is added in the flask of step S1, soak 3～7min of natural flake graphite, add oxidant, stirring 30
～50min, obtains product, and wherein the quality of natural flake graphite and the volume ratio of intercalator are 1：3～1：9, natural squama
Piece graphite is 1 with the mass ratio of oxidant：0.05～1：0.35；
S3, the product that step S2 is obtained is washed to into neutrality, is filtered, 30～50 DEG C of vacuum drying obtain acidifying graphite；
S4, the acidifying graphite that step S3 is obtained is inserted in flask, heating in water bath, keeping temperature is 20 DEG C～30 DEG C；
S5, perchloric acid and acetic acid are separately added in the flask of step S3, are stirred, soak 3～7min of acidifying graphite, then added
Enter oxidant, 30～50min of stirring reaction obtains product, and wherein the quality of acidifying graphite and the volume ratio of perchloric acid are 1:1～
1:4, the quality of acidifying graphite is 1 with the volume ratio of acetic acid:2～1:8, acidifying graphite is 1 with the mass ratio of oxidant:0.05～
1:0.2；
S6, the product that step S5 is obtained is washed to into neutrality, is filtered, 30～50 DEG C of vacuum drying, you can.
2. preparation method according to claim 1, it is characterised in that：Oxidant described in step S2 and step S5 is permanganic acid
One kind in potassium, potassium dichromate, concentrated nitric acid, perchloric acid.
3. preparation method according to claim 1, it is characterised in that：Intercalator described in step S2 is concentrated nitric acid or high chlorine
Acid.
4. the preparation method according to claim 1 or 3, it is characterised in that：The concentration of the perchloric acid is 70%～72%.
5. preparation method according to claim 3, it is characterised in that：The acetic acid concentration is 99.5%.
6. preparation method according to claim 1, it is characterised in that：The quality of natural flake graphite described in step S2 with insert
The volume ratio of layer agent is 1：6～1：7.
7. preparation method according to claim 1, it is characterised in that：Natural flake graphite described in step S2 and oxidant
Mass ratio is 1：0.2～1：0.35.
8. preparation method according to claim 1, it is characterised in that：The quality and perchloric acid of acidifying graphite described in step S5
Volume ratio be 1：1～1：3.
9. preparation method according to claim 1, it is characterised in that：The quality of acidifying graphite described in step S5 and acetic acid
Volume ratio is 1：4～1：5.
10. preparation method according to claim 1, it is characterised in that：The matter of acidifying graphite described in step S5 and oxidant
Amount is than being 1：0.2.
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| CN110371969A (en) * | 2019-08-27 | 2019-10-25 | 哈尔滨市兴显卓科技有限公司 | A kind of smokeless preparation method of preparation method and sulphur-free expanded graphite without discharge expansible graphite |
| CN112520734A (en) * | 2020-12-21 | 2021-03-19 | 中国地质科学院郑州矿产综合利用研究所 | High-quality expandable graphite, preparation method thereof and flexible graphite |
| CN113067002A (en) * | 2021-03-23 | 2021-07-02 | 中国科学院化学研究所 | PEM fuel cell, ball-milling intercalation graphite bipolar plate and preparation method thereof |
| CN113735113A (en) * | 2021-10-21 | 2021-12-03 | 青岛洛唯新材料有限公司 | Expandable graphite and preparation method thereof |
| CN116477620A (en) * | 2023-03-24 | 2023-07-25 | 中国地质大学（武汉） | High-reversible-capacity sodium ion battery anode material, method for preparing same by utilizing large-scale graphite and application thereof |
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| CN110371969A (en) * | 2019-08-27 | 2019-10-25 | 哈尔滨市兴显卓科技有限公司 | A kind of smokeless preparation method of preparation method and sulphur-free expanded graphite without discharge expansible graphite |
| CN112520734A (en) * | 2020-12-21 | 2021-03-19 | 中国地质科学院郑州矿产综合利用研究所 | High-quality expandable graphite, preparation method thereof and flexible graphite |
| CN113067002A (en) * | 2021-03-23 | 2021-07-02 | 中国科学院化学研究所 | PEM fuel cell, ball-milling intercalation graphite bipolar plate and preparation method thereof |
| CN113735113A (en) * | 2021-10-21 | 2021-12-03 | 青岛洛唯新材料有限公司 | Expandable graphite and preparation method thereof |
| CN116477620A (en) * | 2023-03-24 | 2023-07-25 | 中国地质大学（武汉） | High-reversible-capacity sodium ion battery anode material, method for preparing same by utilizing large-scale graphite and application thereof |
| CN116477620B (en) * | 2023-03-24 | 2024-06-04 | 中国地质大学（武汉） | High-reversible-capacity sodium ion battery anode material, method for preparing same by utilizing large-scale graphite and application thereof |
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