CN103964420A - Preparation method of high-purity high-fineness graphite powder - Google Patents
Preparation method of high-purity high-fineness graphite powder Download PDFInfo
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- CN103964420A CN103964420A CN201410154430.9A CN201410154430A CN103964420A CN 103964420 A CN103964420 A CN 103964420A CN 201410154430 A CN201410154430 A CN 201410154430A CN 103964420 A CN103964420 A CN 103964420A
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Abstract
The invention discloses a preparation method of high-purity high-fineness graphite powder, which comprises the following steps: performing irradiation on raw materials of graphite powder by using Gamma ray with a frequency between 10*1018 to 85*1018 Hz for 1 to 2 hours at room temperature; grinding and crushing the irradiated raw materials of the graphite powder to obtain the high-purity high-fineness graphite powder. The preparation method has the benefits that the van der waals force among molecules of the graphite powder is destroyed after the graphite powder is irradiated by using Gamma ray with a certain frequency, so that the frequency of grinding is greatly reduced; grinding impurities are not easy to be introduced, the requirement for preparation of the high-purity graphite powder is met; the preparation method is simple and practicable, and the method is suitable for preparation of the graphite powder with particle size less than 2 micrometers.
Description
The present invention is: application number is 201110294365.6, and the applying date is 2011.9.27, and name is called dividing an application of " preparation method and the application of the high fineness Graphite Powder 99 of high purity ".
Technical field
The present invention relates to the working method of the high fineness powder of a kind of high purity, relate in particular to the preparation method of the high fineness Graphite Powder 99 of a kind of high purity.
Background technology
Superfine graphite powder body material is that the eighties just starts a kind of new and high technology material growing up mid-term, and its purposes is very extensive, can be applicable to the fields such as ink, static carbon dust, coating, fiber, plastics, rubber, electrode.During modernization industry is produced, the common method of preparing superfine graphite powder is mechanical ball milling method and comminution by gas stream.Yet, the shortcoming of mechanical ball milling method is that energy consumption is large, efficiency is low, the particle diameter of the Graphite Powder 99 of producing by this method generally can be lower than 10 microns, and in Graphite Powder 99, easily sneak into impurity, therefore, with the graphite composite powder that mechanical ball magic is pulverized, conventionally can only be applied in some to purity, the less demanding occasion of particle diameter; The shortcoming of comminution by gas stream is to be difficult to graphite composite powder to be crushed to submicron order, and the particle diameter of the Graphite Powder 99 of producing by this method generally also can only reach 10 microns of following, 6 microns of above levels.
Patent 200910069675.0 has been announced a kind of method that improves degree of graphitization of graphite material: graphite material is placed in
60the gamma-ray irradiation source of Co is indoor, in gamma-ray irradiation dose rate, is 0.6 * 10
3gy/h ~ 6 * 10
3gy/h, irradiation dose is 1 * 10
5gy ~ 6 * 10
6under the condition of Gy, graphite material is carried out to gamma-ray irradiation.Provided by the invention is to utilize gamma-rays particle energy is high, penetration power is strong feature at the inside of graphite material initiating activity point for improving the method for degree of graphitization of graphite material, and this active site and material medium is around reacted; Utilize energy that gamma-rays the provides fault location in graphite material inside to produce carbon radicals simultaneously, between carbon radicals, can form more stable chemical bond again, thereby occurring to reset, the structure that makes graphite subsurface defect place forms stable structure more, result is impelled the pitch smaller of graphite wafer, crystallite dimension increases, therefore degree of graphitization improves, and then has improved the conductivity of graphite material.
Patent 200810068381.1 has been announced a kind of preparation method and equipment of Graphite Powder 99: the technical problem that solve is to improve the purity of Graphite Powder 99, reduces costs.Method of the present invention comprises the following steps: through vacuum handling, packs raw material micro mist into plumbago crucible, puts into graphitizing furnace, and thermal treatment, cooling, obtain Graphite Powder 99 product.The Preparation equipment of Graphite Powder 99 consists of the vacuum transportation device being linked in sequence, graphitizing furnace and vacuum discharge device, is placed with plumbago crucible in graphitizing furnace, and graphitizing furnace is connected with inflation system.The present invention compared with prior art, packs plumbago crucible to raw material micro mist into through vacuum handling, and in minimizing treating processes, impurity enters, after thermal treatment, product purity improves greatly, and greying is even, good product consistency, the greying heat treatment efficiency that improves powder body material, technique is simple, cost is low.Yet the step of this method is too complicated, and operation easier is larger, and cost is higher.
For high-energy radiation, process affecting of C-C key also had to some promptings in prior art: the people such as (1) Chen Huiyuan, Ding Zhongmin are prompting " by the high-energy radiation of γ particle, the C-C key in starch polymer, C-O key and c h bond being interrupted " in application > > mono-literary composition in textile sizing at the < < radiation modified starch of < < modern textile technology > > the 1st phase in 2007; (2) Liao Cong, Zhang Xiaoping are pointed out " C-C bond rupture mainly occurs PTFE after high energy (β ray, gamma-rays, high-velocity electrons) irradiation " in < < Advance On Recycle of Waste Polytetrafluoroethylene > > mono-literary composition of < < engineering plastics application > > o. 11th in 2006.(3) people such as Menghe Miao proposes on July 23rd, 2011, the < < gamma ray in < < carbon > > magazine was to effect > > mono-literary composition of carbon-carbon bond: " Raman spectrum analysis being undertaken by Skakalova shows; the wide hurdle of Single Walled Carbon Nanotube grid that is subject to gamma ray radiation has caused the considerable change of D/G ratio in air, and this is in Single Walled Carbon Nanotube, to have a performance of the carbon-carbon bond of fracture.They think under gamma ray, the carbon-carbon bond fracture in Single Walled Carbon Nanotube, once therefore the concentration of defect raises, new key forms again, this just couples together adjacent carbon nanotube ".
Summary of the invention
In view of the defect that above-mentioned prior art exists, the object of the invention is to propose the preparation method of the minimum high-purity graphite powder of a kind of particle diameter.
Object of the present invention, will be achieved by the following technical programs: the preparation method of the high fineness Graphite Powder 99 of a kind of high purity, comprises the steps:
A) at room temperature, frequency of utilization is 10*10
18-85 * 10
18the gamma-rays of Hz irradiates Graphite Powder 99 raw material, and the time length is 1-2 hour;
B) graphite raw material obtaining after step a) processing is ground.
Preferably, also comprise the steps:
C) Graphite Powder 99 described step b) being obtained carries out wet-milling;
D) Graphite Powder 99 after described step c) wet-milling is washed or pickling or alkali cleaning or organic solvent are washed.
E) further grind, the particle of high-purity graphite powder is carried out to shaping, obtain the high fineness Graphite Powder 99 of high purity.
Preferably, described in step b) and step e), grind employing mechanical mill breaking method or plasma breaking method, ultrasonication method, arc process breaking method, explosion method breaking method, described mechanical mill breaking method adopts mechanical grinder or Gas grinding machine to pulverize.
Compared with prior art, beneficial effect of the present invention is:
(1) Graphite Powder 99 after the x ray irradiation x of employing CF, its intermolecular Van der Waals force is destroyed, can greatly reduce the number of times of grinding; Be difficult for introducing grinding impurity, reached the requirement of preparing high-purity graphite powder;
(2) preparation method is simple and practical, can prepare the Graphite Powder 99 that particle diameter is less than 2 microns.
Accompanying drawing explanation
Fig. 1 is the size distribution figure of gained Graphite Powder 99 in embodiment mono-;
Fig. 2 is the size distribution figure of gained Graphite Powder 99 in embodiment bis-;
Fig. 3 a, Fig. 3 b are respectively the Electronic Speculum figure of the Graphite Powder 99 of embodiment mono-and embodiment bis-;
Fig. 4 a, Fig. 4 b are respectively the grind Electronic Speculum figure that condition under grind the Graphite Powder 99 that obtain identical with embodiment bis-with embodiment mono-, and process without any radiation exposure.
Embodiment
Embodiment mono-
The preparation method of the high-purity graphite powder in the present embodiment specifically comprises the steps:
A) at room temperature, frequency of utilization is 10*10
18gamma-rays Graphite Powder 99 raw material is irradiated, the time length is 2 hours;
B) use airflow milling to pulverize having completed the Graphite Powder 99 raw material of step a); As everyone knows, graphite structure cell is to be formed by stacking by the netted plane of carbon atom hexagonal, and it is tabular that the netted plane of each hexagonal is six sides, and frequency is 10*10
18gammairradiation Graphite Powder 99 raw material after, its intermolecular Van der Waals force is destroyed, has broken the structure of graphite wafer intercellular, makes it to become loose and the tabular material of more six sides, thereby is more easily polished;
C) use highly purified water to carry out conventional wet-milling to having completed the Graphite Powder 99 raw material of step b);
D) to having completed the Graphite Powder 99 raw material of step c), carry out pickling, thereby remove, sneak into the metallic impurity in graphite composite powder, the acid solution of using can be hydrochloric acid, sulfuric acid or nitric acid etc.; Then, then remove unnecessary acid solution by pure water rinsing, can certainly wash or alkali cleaning or organic solvent are washed etc.;
E) further grind, the particle of high-purity graphite powder is carried out to shaping.
Figure 1 shows that the size distribution figure that uses the high-purity graphite powder making in the present embodiment, as seen from the figure, the Graphite Powder 99 particle diameter making with the present invention can reach in 2 microns.
Certainly, the step b) in embodiment can be omitted, thereby directly carries out step c) and following step thereof to having completed the Graphite Powder 99 raw material of step a); Step a) and step b) also can be repeatedly, loop, and comprise and put upside down circulation, first Graphite Powder 99 raw material carried out to airflow milling pulverizing or dry grinding is pulverized, and then with rays such as gamma-rays or electron beams, described Graphite Powder 99 raw material irradiated circulation; Certainly, natural graphite powder raw material, also can only perform step a) and step b) if.
Embodiment bis-
The preparation method of the high-purity graphite powder in the present embodiment specifically comprises the steps: that frequency of utilization is 85*10
18gamma-rays Graphite Powder 99 raw material is irradiated, the time length is 2 hours; Other step is identical with embodiment mono-, does not repeat them here.
Figure 2 shows that the size distribution figure that uses the high-purity graphite powder making in the present embodiment, as seen from the figure, the Graphite Powder 99 particle diameter making with the present invention can reach in 2 microns.
Adopt the gamma-rays of the correlated frequency disclosing in embodiment mono-and two to irradiate Graphite Powder 99 raw material, time length is 1 hour, also can reach the size distribution figure of the Graphite Powder 99 as disclosed in Fig. 1 and Fig. 2, because its preparation method is all identical with embodiment mono-and two with experimental result, therefore do not repeat them here.
Graphite Powder 99 raw material in various embodiments of the present invention also can use coke powder, carbon black, coal dust, gac etc. to substitute, and can obtain corresponding high purity powdered form like this by method of the present invention.The Graphite Powder 99 that technology in the present invention is produced (dilator) or carbon dust can be used for (comprising the coke of refinery coke, pitch coke, high purity coal dust, needle coke, high-carbon and high-temperature calcination thing, the dilator of above material) preparation of coating, plastics, rubber, fiber, insulating cotton, power supply and battery.
It should be noted that, the step that adopts CF radiation exposure Graphite Powder 99 raw material in the present invention is mainly to destroy its intermolecular Van der Waals force, making it to be more easily polished, and improves the smashing capability of graphite material.The particle diameter comparison diagram directly not grinding through gammairradiation that grind again after gammairradiation and Fig. 4 a-Fig. 4 b specifically disclosing in conjunction with Fig. 3 a-Fig. 3 b discloses, illustrates the size adopting after identical grinding condition.
For example: the preparation process of the graphite particle in Fig. 3 a is: a) at room temperature, frequency of utilization is 10*10
18gamma-rays Graphite Powder 99 raw material is irradiated, the time length is 2 hours; B) adopt airflow milling, grinding condition: high velocity air (400m/s), 8 kilograms of air pressure, 10 cubes of gases; The particle diameter of the graphite particle in Fig. 3 a obtaining is 2um(D90), output is 22 kilograms per hour.Corresponding, the preparation process of the graphite particle in Fig. 4 a is for adopting airflow milling, grinding condition: high velocity air (400m/s), 8 kilograms of air pressure, 10 cubes of gases; The particle diameter of the graphite particle in Fig. 4 a obtaining is 10um(D90), output is 18 kilograms per hour.
Same, Fig. 3 b is that the part powdered graphite of second batch is first 85*10 through the frequency of the second embodiment
18the Electronic Speculum figure of the graphite particle that obtains after grinding again after 2 hours of gammairradiation, Fig. 4 b is the Electronic Speculum figure of the graphite particle that obtains after the part powdered graphite of second batch directly grinds.Both adopt identical grinding condition: airflow milling, high velocity air (400m/s), 8 kilograms of air pressure, 10 cubes of gases.Accordingly, the particle diameter of the graphite particle in Fig. 3 b is 2um(D90), output is 22 kilograms per hour.The particle diameter of the graphite particle in Fig. 4 b is 10um(D90), output is 18 kilograms per hour.
In above-mentioned all Electronic Speculum figure, draw, the graphite particle obtaining after grinding again after the gammairradiation of CF is generally in 2 um, and graphite particle appearance is mellow and full, can not need to carry out Shape correction; And the graphite particle obtaining after directly grinding is generally in about 10um, and graphite particle appearance is sharp-pointed, and sequence is chaotic.Therefore can verify the validity that the gammairradiation of CF grinds for graphite particle, and the step of radiation exposure Graphite Powder 99 raw material in the graphitizing process of prior art is mainly at the conductivity that improves graphite material, and in prior art all without any prompting radiation exposure Graphite Powder 99 raw material can improve the smashing capability of graphite material.Therefore the present invention has obtained beyond thought effect.
The present invention still has numerous embodiments, such as gamma-rays, also can interrupt class carbon-carbon bond (such as silicon, selenium etc.), CH key, its intermolecular Van der Waals force is destroyed, so the powder stock that this dvielement forms equally also can obtain high purity powdered form by method of the present invention.Described grinding except adopting mechanical mill breaking method, can also adopting plasma breaking method, ultrasonication method, arc process breaking method, explosion method breaking method etc.All employing equivalents or equivalent transformation and all technical schemes of forming, within all dropping on protection scope of the present invention.
Claims (4)
1. a preparation method for the high fineness Graphite Powder 99 of high purity, is characterized in that, comprises the steps:
A) at room temperature, frequency of utilization is 10*10
18-85 * 10
18the gamma-rays of Hz irradiates Graphite Powder 99 raw material, and the time length is 1-2 hour;
B) graphite raw material obtaining after step a) processing is ground.
2. the preparation method of the high fineness Graphite Powder 99 of a kind of high purity according to claim 1, is characterized in that, also comprises the steps:
C) Graphite Powder 99 described step b) being obtained carries out wet-milling;
D) Graphite Powder 99 after described step c) wet-milling is washed or pickling or alkali cleaning or organic solvent are washed.
3. the preparation method of the high fineness Graphite Powder 99 of a kind of high purity according to claim 2, is characterized in that, also comprises the steps: e) further grind, the particle of high-purity graphite powder is carried out to shaping, obtain the high fineness Graphite Powder 99 of high purity.
4. the preparation method of the high fineness Graphite Powder 99 of a kind of high purity according to claim 3, it is characterized in that: described in step b) and step e), grind employing mechanical mill breaking method or plasma breaking method, ultrasonication method, arc process breaking method, explosion method breaking method, described mechanical mill breaking method adopts mechanical grinder or Gas grinding machine to pulverize.
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|---|---|---|---|
| CN201410154430.9A CN103964420A (en) | 2011-09-27 | 2011-09-27 | Preparation method of high-purity high-fineness graphite powder |
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Citations (4)
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|---|---|---|---|---|
| US4921687A (en) * | 1987-11-28 | 1990-05-01 | Tohoku University | Method of making high-orientation sheet-like graphite by using laminar compound |
| CN1244495A (en) * | 1998-08-10 | 2000-02-16 | 张小宁 | Preparation of superfine graphite powder |
| CN1378976A (en) * | 2002-05-17 | 2002-11-13 | 贵州航天纳米科技有限责任公司 | Process for preparing nano graphite carbon powder from nano graphite sol |
| CN101607706A (en) * | 2009-07-10 | 2009-12-23 | 天津工业大学 | A kind of method that is used to improve degree of graphitization of graphite material |
-
2011
- 2011-09-27 CN CN201410154430.9A patent/CN103964420A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4921687A (en) * | 1987-11-28 | 1990-05-01 | Tohoku University | Method of making high-orientation sheet-like graphite by using laminar compound |
| CN1244495A (en) * | 1998-08-10 | 2000-02-16 | 张小宁 | Preparation of superfine graphite powder |
| CN1378976A (en) * | 2002-05-17 | 2002-11-13 | 贵州航天纳米科技有限责任公司 | Process for preparing nano graphite carbon powder from nano graphite sol |
| CN101607706A (en) * | 2009-07-10 | 2009-12-23 | 天津工业大学 | A kind of method that is used to improve degree of graphitization of graphite material |
Non-Patent Citations (2)
| Title |
|---|
| MENGHE MIAO: "Electrical conductivity of pure carbon nanotube yarns", 《CARBON》, vol. 49, no. 12, 11 May 2011 (2011-05-11), pages 3755 - 3761, XP028238666, DOI: 10.1016/j.carbon.2011.05.008 * |
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Application publication date: 20140806 |