CN102320596A - Preparation method of fine-flake expanded graphite - Google Patents
Preparation method of fine-flake expanded graphite Download PDFInfo
- Publication number
- CN102320596A CN102320596A CN201110195890A CN201110195890A CN102320596A CN 102320596 A CN102320596 A CN 102320596A CN 201110195890 A CN201110195890 A CN 201110195890A CN 201110195890 A CN201110195890 A CN 201110195890A CN 102320596 A CN102320596 A CN 102320596A
- Authority
- CN
- China
- Prior art keywords
- graphite
- preparation
- expanded graphite
- flake
- crystalline flake
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Carbon And Carbon Compounds (AREA)
Abstract
The invention relates to a preparation method of fine-flake expanded graphite. The preparation method comprises the following steps: 1) uniformly mixing flake graphite with potassium permanganate, adding liquid perchloric acid, and then reacting at the temperature of 35-40 DEG C while stirring for 60-120 minutes to obtain a mixture; 2) adding clean water to the mixture, washing until the pH value is 5.5-6.5, then dewatering, and drying to obtain intercalated flake graphite; and 3) finally placing the intercalated flake graphite in a muffle furnace, and carrying out instantaneous expansion. The preparation method provided by the invention has the beneficial effects that: in the method, flake graphite with the size of minus 80 to 200 meshes is used to produce expanded graphite, thus expanded graphite with higher expansion rate (250-650mL/g) can be prepared; and the prepared expanded graphite has physical and chemical properties of graphite as well as plasticity and excellent sealing property, and is an excellent nonmetal sealing, flame-retardant, antistatic, electroconductive, heat-conducting, anticorrosive, wave-absorbing and electromagnetic shielding material.
Description
Technical field
The present invention relates to a kind of preparation method of flake-shaped expanded graphite, especially have very high expansion multiplying power.
Background technology
At present; Preparation high magnification expanded graphite all adopts LG80-99 (i.e. 80 orders; Carbon containing 99%) flaky graphite; The expanded graphite of this flaky graphite preparation is much better than conventional seals materials such as asbestos, rubber, tetrafluoroethylene, metal owing to have characteristics such as snappiness, rebound resilience, autohension, low density and anisotropy as its over-all properties of sealing material.But use flaky graphite very poor as the Antistatic Paint surface aesthetic property of the expanded graphite making of feedstock production, color and luster is bad; In addition, along with high-quality flaky graphite resource is fewer and feweri, partly replacing flaky graphite seems particularly important thereby thin crystalline flake graphite is prepared into the high magnification expanded graphite.Because the granularity characteristics of thin crystalline flake graphite; If adopt chemical oxidization method to use traditional oxygenant, intercalator such as ydrogen peroxide 50, potassium permanganate, nitric acid, sulfuric acid, iron(ic)chloride etc. to LG (80～+ 200)-99 (order～+ 200 orders promptly-80; Carbon containing 99%) thin crystalline flake graphite carries out intercalation processing, then can only make very low (50-80ml/g) expanded graphite of expansion multiplying power.
Summary of the invention
The present invention proposes the method that a kind of thin crystalline flake graphite prepares the high magnification expanded graphite for the not high problem of flake-shaped expanded graphite expansion multiplying power that solves above-mentioned prior art existence; The expansible black lead that adopts the preparation of this method can get the expanded graphite that expansion multiplying power is 250-650ml/g after expanded.
The present invention solves the problems of the technologies described above the technical scheme that is adopted: the preparation method of flake-shaped expanded graphite includes following steps:
1) with crystalline flake graphite and potassium permanganate uniform mixing; The adding weight of potassium permanganate is the 5-10% of graphite; Add liquid perchloric acid again; Wherein the mass and size proportioning of crystalline flake graphite and perchloric acid is 2g:1.5-3ml, is reaction 60-120min under 35-40 ℃ and the agitation condition in temperature then, obtains mixture;
2) mixture that step 1) is obtained add clear water wash to the pH value for 5.5-6.5, dewater then, drying obtains intercalation crystalline flake graphite, it contains the moisture weight percent content is 8-15%;
3) at last with step 2) crystalline flake graphite of intercalation that obtains puts into retort furnace and carries out instantaneous expansion, get final product expanded graphite.
Press such scheme, described crystalline flake graphite size is-80 orders～+ 200 orders, and its carbon content is 99%, the mass percent meter.
Press such scheme, the described instantaneous expansion temperature of reaction of step 3) is 900-950 ℃, and the instantaneous expansion reaction times is 10-30 second.
Press such scheme, the expansion multiplying power of expanded graphite is 250-650ml/g.
The present invention with respect to the beneficial effect of prior art is: the problem of utilizing that has solved-80 orders～+ 200 order crystalline flake graphites; Utilize present method to adopt-80 orders～+ 200 order crystalline flake graphites to produce expanded graphite; Overcome traditional method NOx, SOx gas pollution to environment; Can prepare the expanded graphite with very high expansion multiplying power (250-650mL/g), solving simultaneously with 80 order crystalline flake graphites is that the expanded graphite of the feedstock production Antistatic Paint surface aesthetic property of making is poor, the problem that color and luster is bad; But the flaky graphite resource of saves valuable also; Prepared expanded graphite has the physico-chemical property of graphite, through the raising to particulate crystalline flake graphite expansion multiplying power, has greatly widened the Application Areas of particulate crystalline flake graphite; Have plasticity-and good sealing characteristics in addition, be good nonmetal sealing, fire-retardant, anti-electrostatic, conduction, heat conduction, anticorrosive, inhale ripple and electromagnetic shielding material.
Description of drawings
Fig. 1 is SEM (200 times) photo of embodiment 2 raw material crystalline flake graphites;
Fig. 2 is embodiment 2 SEM of intercalation crystalline flake graphite (200 a times) photo;
The SEM of the expanded graphite that Fig. 3 obtains for embodiment 2 (Fig. 3 a and Fig. 3 b are respectively 1000 times and 200 times) photo.
Embodiment
Further introduce the present invention through embodiment below, but embodiment can not be construed as limiting the invention.
Embodiment 1
Be-80 orders～+ 100 orders with the crystalline flake graphite size at first, its carbon content is 99%, mass percent meter (being LG (80～+ 100)-99) the same solid potassium permanganate of crystalline flake graphite (10g) (0.8g, purity 99.7%; The mass percent meter) in beaker, mix, under agitation condition, adding 10ml concentration in the beaker is the liquid perchloric acid of 70-72% (mass percent), is 35 ℃ and continuous agitation conditions reaction 90min down in temperature; Then the gained mixture is added the clear water washing; Until its pH value is 6, and dewatering, dry (under 50 ℃) to moisture weight percent content again is 10%, obtains intercalation crystalline flake graphite; Then take out 1.2g graphite therein and put into crucible (crucible has been heated to 930 ℃); Fast crucible being put into temperature again is 930 ℃ of high temperature retort furnaces, has nothing to do with fire door, till graphite no longer expands; Take out crucible, can make the expanded graphite that expansion multiplying power is 650ml/g at once.
Embodiment 2
Be-100 orders～+ 150 orders with the crystalline flake graphite size at first, its carbon content is 99%, mass percent meter (being LG (100～+ 150)-99) the same solid potassium permanganate of crystalline flake graphite (10g) (1g, purity 99.7%; The mass percent meter) in beaker, mix, under agitation condition, adding 12ml concentration in the beaker is the liquid perchloric acid of 70-72% (mass percent), is 35 ℃ and continuous agitation conditions reaction 90min down in temperature; Then the gained mixture is added the clear water washing; Until its pH value is 6, and dewatering, dry (under 50 ℃) to moisture weight percent content again is 12%, obtains intercalation crystalline flake graphite; Then take out 1.2g graphite therein and put into crucible (crucible has been heated to 930 ℃); Fast crucible being put into temperature again is 930 ℃ of high temperature retort furnaces, has nothing to do with fire door, till graphite no longer expands; Take out crucible, can make the expanded graphite that expansion multiplying power is 500ml/g at once.
Embodiment 3
At first just the crystalline flake graphite size is-150 orders～+ 200 orders, and its carbon content is 99%, mass percent meter (being LG (150～+ 200)-99) the same solid potassium permanganate of crystalline flake graphite (10g) (1g, purity 99.7%; The mass percent meter) in beaker, mix, under agitation condition, adding 15ml concentration in the beaker is the liquid perchloric acid of 70-72% (mass percent), is 35 ℃ and continuous agitation conditions reaction 90min down in temperature; Then the gained mixture is added the clear water washing; Until its pH value is 6, and dewatering, dry (under 50 ℃) to moisture weight percent content again is 12%, obtains intercalation crystalline flake graphite; Then take out 1.2g graphite therein and put into crucible (crucible has been heated to 930 ℃); Fast crucible being put into temperature again is 930 ℃ of high temperature retort furnaces, has nothing to do with fire door, till graphite no longer expands; Take out crucible, can make the expanded graphite that expansion multiplying power is 250ml/g at once.
As shown in Figure 3, learn that through electromicroscopic photograph research the graphite carbon-coating along being that the C direction of principal axis expands perpendicular to the graphite microcrystal bedding angle, produces a large amount of spaces as accordion to expanded graphite; Further investigation shows: expand in two ways along the C direction of principal axis, or expand with balanced way along the C direction of principal axis, or be fan-shaped mode along the C direction of principal axis and expand.
Claims (4)
1. the preparation method of flake-shaped expanded graphite includes following steps:
1) with crystalline flake graphite and potassium permanganate uniform mixing; The adding weight of potassium permanganate is the 5-10% of graphite; Add liquid perchloric acid again; Wherein the mass and size proportioning of crystalline flake graphite and perchloric acid is 2g:1.5-3ml, is reaction 60-120min under 35-40 ℃ and the agitation condition in temperature then, obtains mixture;
2) mixture that step 1) is obtained add clear water wash to the pH value for 5.5-6.5, dewater then, drying obtains intercalation crystalline flake graphite, it contains the moisture weight percent content is 8-15%;
3) at last with step 2) crystalline flake graphite of intercalation that obtains puts into retort furnace and carries out instantaneous expansion, get final product expanded graphite.
2. by the preparation method of the described flake-shaped expanded graphite of claim 1, it is characterized in that described crystalline flake graphite size is-80 orders～+ 200 orders, its carbon content is 99%, the mass percent meter.
3. by the preparation method of claim 1 or 2 described flake-shaped expanded graphites, it is characterized in that the described instantaneous expansion temperature of reaction of step 3) is 900-950 ℃, the instantaneous expansion reaction times is 10-30 second.
4. by the preparation method of the described flake-shaped expanded graphite of claim 3, the expansion multiplying power that it is characterized in that expanded graphite is 250-650ml/g.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110195890A CN102320596A (en) | 2011-07-13 | 2011-07-13 | Preparation method of fine-flake expanded graphite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110195890A CN102320596A (en) | 2011-07-13 | 2011-07-13 | Preparation method of fine-flake expanded graphite |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102320596A true CN102320596A (en) | 2012-01-18 |
Family
ID=45448476
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110195890A Pending CN102320596A (en) | 2011-07-13 | 2011-07-13 | Preparation method of fine-flake expanded graphite |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102320596A (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105502360A (en) * | 2015-12-25 | 2016-04-20 | 燕山大学 | Preparation method of sulfur-free expansible graphite |
| CN106304789A (en) * | 2016-08-30 | 2017-01-04 | 郑州人造金刚石及制品工程技术研究中心有限公司 | A kind of NEW TYPE OF COMPOSITE fin and preparation method thereof |
| CN106299364A (en) * | 2016-10-17 | 2017-01-04 | 山西大学 | A kind of lithium ion battery preparation method containing manganese anthelmintic graphite |
| CN106505219A (en) * | 2016-11-11 | 2017-03-15 | 攀钢集团攀枝花钢铁研究院有限公司 | Vanadium redox flow battery electrode component |
| CN106672962A (en) * | 2016-12-16 | 2017-05-17 | 北京鼎臣超导科技有限公司 | Preparation method of expanded graphite |
| CN106744926A (en) * | 2016-12-16 | 2017-05-31 | 北京鼎臣超导科技有限公司 | A kind of preparation method of expanded graphite |
| CN108641173A (en) * | 2018-05-16 | 2018-10-12 | 辽宁大学 | A kind of preparation method of the linear low density polyethylene material with high flame-retardant property |
| CN108862271A (en) * | 2018-09-28 | 2018-11-23 | 辽宁大学 | A kind of expansible graphite preparation method of proportion optimizing intercalator |
| CN112708229A (en) * | 2020-12-24 | 2021-04-27 | 浙江国泰萧星密封材料股份有限公司 | Preparation method of high-temperature-resistant mud-shaped filler |
| CN114790000A (en) * | 2022-04-19 | 2022-07-26 | 宁波信远炭材料有限公司 | High-temperature-resistant sealing material based on expanded graphite and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1239071A (en) * | 1998-06-17 | 1999-12-22 | 攀枝花大学 | Process for preparing flake-shaped expanded 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 |
| CN1462724A (en) * | 2003-04-30 | 2003-12-24 | 中国科学院山西煤炭化学研究所 | Method for preparing expanded graphite without sulphur |
| US20040000735A1 (en) * | 2002-06-28 | 2004-01-01 | Graftech Inc. | Partially expanded, free flowing, acid treated graphite flake |
-
2011
- 2011-07-13 CN CN201110195890A patent/CN102320596A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1239071A (en) * | 1998-06-17 | 1999-12-22 | 攀枝花大学 | Process for preparing flake-shaped expanded graphite |
| US20040000735A1 (en) * | 2002-06-28 | 2004-01-01 | Graftech Inc. | Partially expanded, free flowing, acid treated graphite flake |
| 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 |
| CN1462724A (en) * | 2003-04-30 | 2003-12-24 | 中国科学院山西煤炭化学研究所 | Method for preparing expanded graphite without sulphur |
Non-Patent Citations (1)
| Title |
|---|
| 刘国钦等: "利用细鳞片石墨制备膨胀石墨的研究", 《新型炭材料》 * |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105502360A (en) * | 2015-12-25 | 2016-04-20 | 燕山大学 | Preparation method of sulfur-free expansible graphite |
| CN106304789A (en) * | 2016-08-30 | 2017-01-04 | 郑州人造金刚石及制品工程技术研究中心有限公司 | A kind of NEW TYPE OF COMPOSITE fin and preparation method thereof |
| CN106299364A (en) * | 2016-10-17 | 2017-01-04 | 山西大学 | A kind of lithium ion battery preparation method containing manganese anthelmintic graphite |
| CN106299364B (en) * | 2016-10-17 | 2019-07-23 | 山西大学 | A kind of preparation method of the lithium ion battery graphite of worm containing manganese |
| CN106505219B (en) * | 2016-11-11 | 2019-03-15 | 攀钢集团攀枝花钢铁研究院有限公司 | Vanadium redox flow battery electrode component |
| CN106505219A (en) * | 2016-11-11 | 2017-03-15 | 攀钢集团攀枝花钢铁研究院有限公司 | Vanadium redox flow battery electrode component |
| CN106744926A (en) * | 2016-12-16 | 2017-05-31 | 北京鼎臣超导科技有限公司 | A kind of preparation method of expanded graphite |
| CN106744926B (en) * | 2016-12-16 | 2019-01-22 | 北京鼎臣超导科技有限公司 | A kind of preparation method of expanded graphite |
| CN106672962A (en) * | 2016-12-16 | 2017-05-17 | 北京鼎臣超导科技有限公司 | Preparation method of expanded graphite |
| CN108641173A (en) * | 2018-05-16 | 2018-10-12 | 辽宁大学 | A kind of preparation method of the linear low density polyethylene material with high flame-retardant property |
| CN108862271A (en) * | 2018-09-28 | 2018-11-23 | 辽宁大学 | A kind of expansible graphite preparation method of proportion optimizing intercalator |
| CN112708229A (en) * | 2020-12-24 | 2021-04-27 | 浙江国泰萧星密封材料股份有限公司 | Preparation method of high-temperature-resistant mud-shaped filler |
| CN114790000A (en) * | 2022-04-19 | 2022-07-26 | 宁波信远炭材料有限公司 | High-temperature-resistant sealing material based on expanded graphite and preparation method thereof |
| CN114790000B (en) * | 2022-04-19 | 2024-04-02 | 宁波信远炭材料有限公司 | High-temperature-resistant sealing material based on expanded graphite and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102320596A (en) | Preparation method of fine-flake expanded graphite | |
| Lee et al. | Photocatalytic hydrogen evolution from water splitting using Cu doped ZnS microspheres under visible light irradiation | |
| Shi et al. | Rooting MnO2 into protonated g-C3N4 by intermolecular hydrogen bonding for endurable supercapacitance | |
| CN107362818A (en) | Nitrogen phosphorus codope carbon coating transition metal diphosphide liberation of hydrogen catalyst and preparation method | |
| Xiong et al. | Facile single-step ammonia heat-treatment and quenching process for the synthesis of improved Pt/N-graphene catalysts | |
| CN101456553B (en) | Chemical processing method for preparing high quality inflatable graphite | |
| CN102616772B (en) | Method for preparing waste recovered graphite powder into graphene | |
| JP7122342B2 (en) | Silicon-Nitrogen Co-Doped Graphene Catalyst Material, Method for Making Same, and Use Thereof | |
| CN110228797A (en) | A kind of method that low cost prepares two-dimentional molybdenum nitride or tungsten nitride nanometer sheet | |
| Islam et al. | A sustainable approach for tungsten carbide synthesis using renewable biopolymers | |
| Mishra et al. | Phosphorous, boron and sulfur doped g-C3N4 nanosheet: Synthesis, characterization, and comparative study towards photocatalytic hydrogen generation | |
| CN103476226A (en) | Preparation method of high-heat-conductivity graphite radiating fin | |
| Zhou et al. | The impact of nitrogen doping and reduced-niobium self-doping on the photocatalytic activity of ultra-thin Nb 3 O 8− nanosheets | |
| CN108046392B (en) | Sewage treatment agent | |
| CN103395769A (en) | Preparation method of porous carbon material based on ionic heat process | |
| CN103265827B (en) | Method for intercalating and organically modifying kaolin by cetyl trimethyl ammonium bromide | |
| CN112320797A (en) | Preparation method of activated carbon for desulfurization of tar hydrogenation product | |
| Sun et al. | Flexible, recoverable, and efficient photocatalysts: MoS2/TiO2 heterojunctions grown on amorphous carbon-coated carbon textiles | |
| CN102532539A (en) | Preparation method of one-dimensional conductive polypyrrole/ concave-convex rod nanameter composite material | |
| CN110273162A (en) | A kind of iron/cobalt/nickel nitrogen coupling C-base composte material and its application | |
| Ou et al. | Ethanol-assisted molten salt synthesis of Bi4Ti3O12/Bi2Ti2O7 with enhanced visible light photocatalytic performance | |
| Shao et al. | Atomically dispersed calcium as solid strong base catalyst with high activity and stability | |
| Zheng et al. | Tuning the morphology and pyrolysis process of rare-earth Gd-doped prussian blue derivatives for electromagnetic wave absorption and anti-corrosion performance | |
| Li et al. | Effect of original crystal size of kaolinite on the formation of intercalation compounds of coal-measure kaolinite | |
| CN108735525A (en) | A kind of graphene/carbon point/manganese dioxide composite material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20120118 |