CN102126721B - Purification and graphitization method of graphite material - Google Patents
Purification and graphitization method of graphite material Download PDFInfo
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- CN102126721B CN102126721B CN2011101065438A CN201110106543A CN102126721B CN 102126721 B CN102126721 B CN 102126721B CN 2011101065438 A CN2011101065438 A CN 2011101065438A CN 201110106543 A CN201110106543 A CN 201110106543A CN 102126721 B CN102126721 B CN 102126721B
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Abstract
The invention discloses a purification and graphitization method of a graphite material, aiming at solving the technical problems of improving the quality of the graphite material, saving energy and reducing cost. The method comprises the following steps: putting a graphite product or a carbon product in a graphite crucible in a furnace body; heating to 900-1700 DEG C, and then introducing nitrogen or argon; continuing to heat to 1000-1950 DEG C, introducing chlorine and then continuing to rising the temperature to 1400-2300 DEG C; simultaneously, introducing bromine or a fluorine-containing gas, heating to 1800-3300 DEG C and then stopping heating; introducing the chlorine until the temperature is reduced to below 1000-2000 DEG C; and feeding nitrogen or argon lasting for more than 0-15 hours. Compared with the prior art, the ash content of the obtained graphite product is less than 0.00011%; electrical energy consumption is reduced; and the method has the advantages that the process is simple, the cost is low, the quality of the graphite product is stable, and energy is saved.
Description
Technical field
The present invention relates to the working method of a kind of working method of non-metallic material, particularly a kind of graphite material.
Background technology
Graphite material has wide market outlook in new technical field such as the energy, environmental protection, information, traffic, national defence.Such as the electrode materials of battery, the bipolar plates of fuel cell, flexible graphite sealing material, the coated material of electronic message unit, the stealth material of military equipment etc.The deep processed product of graphite material often has higher added value, but the deep processing method the highest link that is requirement.Graphitization technique is one of method important in the deep processing.Domestic main graphitization technique has serial graphitized and acheson graphite at present.After the eighties in 20th century, cascade graphitizing furnaces occurred, cause the concern of countries in the world with its advanced technology, it nearly all is the situation that adopts Acheson's type graphitizing furnace that its emergence has been broken in the greying production.Yet cascade graphitizing furnaces is only suitable for the production of single large specification product, and technology is comparatively complicated, does not generally have the device that passes into gas is set, and can't purify to finished product.So Acheson's type graphitizing furnace can not be substituted fully, and will in greying is produced, use, particularly occupied certain status in middle-size and small-size charcoal ink factory.Yet only there are cascade graphitizing furnaces and Acheson's type graphitizing furnace can't satisfy the needs of scale operation graphite.Especially prepare high-end lithium ion battery negative material, high purity graphite, graphite fibre etc., it is higher to graphited requirement, and the method for graphitizing of prior art can't satisfy it to the requirement of graphite material.
Summary of the invention
The purifying and the method for graphitizing that the purpose of this invention is to provide a kind of graphite material, the technical problem that solve are the quality that improves graphite material, energy-conservation and reduction cost.
The present invention is by the following technical solutions: a kind of purifying of graphite material and method for graphitizing may further comprise the steps: the plumbago crucible of one, graphite product or carbon product being put into body of heater; Two, the speed with 5～300 ℃/min heats up, and the temperature of plumbago crucible reaches 900～1700 ℃ in stove, with 1～5m
3The flow of/h passes into nitrogen or argon gas; Three, the speed with 5～300 ℃/min continues to heat up, and when temperature reaches 1000～1950 ℃, changes into 1～5m
3The flow of/h passes into chlorine; Four, continue again to be warming up to 1400～2300 ℃ with the speed of 5～300 ℃/min, simultaneously with 1～5m
3The flow of/h passes into bromine gas or fluoro-gas, and fluoro-gas is freonll-11 or freon, until temperature stopped heating when rising to 1800～3300 ℃ changes with 1～5m again
3The flow of/h passes into chlorine and is reduced to below 1000～2000 ℃ to temperature, again with 0.1～5m
3The flow of/h is sent into nitrogen or argon gas, keeps obtaining graphite product greater than 0 to 15h.
Temperature of the present invention is reduced to below 1000～2000 ℃, again with 0.1～5m
3The flow of/h is sent into nitrogen or argon gas, keeps naturally cooling to below 100 ℃ greater than 0 to 15h.
The present invention is to the graphite product screening, except magnetic.
Graphite product of the present invention is that fixed carbon content is at the natural graphite powder more than 85%, graphous graphite powder, microlite ink powder, coking coal, coke or Graphite Electrodes, carbon product are that fixed carbon content is at the carbon nanotube more than 85%, carbon fiber, needle coke or refinery coke.
Plumbago crucible of the present invention is 30 to 90 serial connections, and each plumbago crucible capacity is 50 to 300 liters.
Connect the distribution of current plate of graphite matter between the stove end electrode at body of heater of the present invention two ends, connect plumbago crucible between the distribution of current plate.
Plumbago crucible of the present invention is connected in series by pad, and pad is smeared be used to the contact cream that improves the end face electrical contact performance.
The used logical electrically heated transformer capacity of body of heater of the present invention is for being not less than 1.6 ten thousand KVA, and voltage adjusting range is at 15V to 300V.
Be filled with the thick metallurgical coke of 300～1000mm or refinery coke insulation material between plumbago crucible of the present invention and the body of heater, body of heater is made of the furnace wall on furnace bottom and the furnace bottom, bottom of furnace body pack into 200～1000mm thick metallurgical coke or refinery coke furnace burdening, metallurgical coke or coke grain are to 50mm greater than 0.
The end of the present invention, be provided with the ventilation carbon tube, one termination of ventilation graphite enters in the body of heater, the other end connects chlorine pot, fluoro-gas tank, nitrogen pot, argon tanks and bromine gas tank through a collecting pipe, described chlorine pot, fluoro-gas tank, nitrogen pot, argon tanks and bromine gas tank are provided with valve and under meter, and collecting pipe is five to advance a connecting tube that outes.
The present invention compared with prior art; during greying, pass into the protection of rare gas element or purifying gas, directly the graphite material in the stove is heated; material is heated evenly internally; the graphite product ash oontent that obtains is less than 0.00011%, and iron content is below 5ppm, and the pH value is 4.5～10.0; interlamellar spacing is at 0.3354～0.3365nm; grain-size Lc (002) is 200～1000nm, and magnetic substance content is less than 0.1ppm, and real density is at 2.20～2.26g/cm
3Method for graphitizing of the present invention adopts the plumbago crucible serial connection, is filled with protection of inert gas in stove; the graphited while; pass into purifying gas, greying or carbonizing treatment, purification process are united two into one, electric current is evenly distributed in electrode and graphite material during heating; greatly shorten the production cycle; simultaneously can avoid using resistance material to add thermogenesis and transferring heat, reduce power consumption, have that technique is simple, a graphite products steady quality, energy-conservation, advantage cheaply.
Description of drawings
Fig. 1 is the equipment structure chart that the present invention adopts.
Fig. 2 is the A-A view of Fig. 2.
Fig. 3 is the SEM figure after embodiment 1 graphitization technique is processed.
Embodiment
Below in conjunction with drawings and Examples the present invention is described in further detail.Purifying of the present invention and method for graphitizing, adopt following steps:
One, graphite product or carbon product are put into the plumbago crucible of body of heater, graphite product is that fixed carbon content is at the natural graphite powder more than 85%, graphous graphite powder, microlite ink powder, coking coal, coke or Graphite Electrodes, carbon product are that fixed carbon content is at the carbon nanotube more than 85%, carbon fiber, needle coke or refinery coke.As depicted in figs. 1 and 2, the distribution of current plate 3 that connects graphite matter between the stove end electrode 2 at body of heater two ends, consecutive connects 30 to 90 plumbago crucibles 4 between the distribution of current plate 3, stove end electricity level 2 two ends are thrustors 1, each plumbago crucible 4 capacity is 50 to 300 liters, plumbago crucible 4 is by pad 5 serial connections, pad 5 is coated be used to the contact cream that improves the end face electrical contact performance, the used logical electrically heated transformer capacity of body of heater is for being not less than 1.6 ten thousand KVA, voltage adjusting range is at 15V to 300V, be filled with the thick metallurgical coke of 300～1000mm or refinery coke 9 insulation materials between plumbago crucible 4 and the body of heater, body of heater is made of the furnace wall 6 on furnace bottom 8 and the furnace bottom 8, bottom of furnace body pack into 200～1000mm thick metallurgical coke or refinery coke 9 furnace burdenings, metallurgical coke or refinery coke 9 granularities are to 50mm greater than 0, furnace bottom 8 is provided with ventilation carbon tube 7, and a termination of ventilation carbon tube 7 enters in the body of heater, and the other end connects chlorine pot 10 through a collecting pipe, fluoro-gas tank 11, nitrogen pot 12, argon tanks 13 and bromine gas tank 14.Chlorine pot 10, contain fluoro-gas tank 11, nitrogen pot 12, argon tanks 13 and bromine gas tank 14 and be provided with valve and under meter, collecting pipe is five to advance a connecting tube that outes.
Two, the speed with 5～300 ℃/min heats up, and the temperature of plumbago crucible reaches 900～1700 ℃ in stove, with 1～5m
3The flow of/h passes into nitrogen or argon gas.
Three, the speed with 5～300 ℃/min continues to heat up, and when temperature reaches 1000～1950 ℃, changes into 1～5m
3The flow of/h passes into chlorine.
Four, continue again to be warming up to 1400～2300 ℃ with the speed of 5～300 ℃/min, simultaneously with 1～5m
3The flow of/h passes into bromine gas or fluoro-gas, and fluoro-gas is freonll-11 or freon, send electrically heated until temperature stops greying when rising to 1800～3300 ℃, changes with 1～5m again
3The flow of/h passes into chlorine and is reduced to below 1000～2000 ℃ to temperature, again with 0.1～5m
3The flow of/h is sent into nitrogen or argon gas, keeps greater than 0 to 15h time.
Five, naturally cool to below 100 ℃.
Six, sieve, remove magnetic and obtain graphite product.The ash oontent of graphite product is less than 0.00011%, and iron content is below 5ppm, and the pH value is 4.5～10.0, interlamellar spacing is at 0.3354～0.3365nm, grain-size Lc (002) is 200-1000nm, and magnetic substance content is less than 0.1ppm, and real density is at 2.20～2.26g/cm
3
Method of the present invention directly heats the plumbago crucible of charging, need not heat stopping composition, reduces the power consumption that causes because of the resistance material heat.Rate of heating is fast, and current density is large, and stove inner core temperature is high, and the degree of graphitization of product is high, the quality product stable homogeneous.
Many plumbago crucible serial connections of the present invention, be different from conventional serial graphitized mode, not only graphitization temperature is high, and can in graphitizing process, pass into rare gas element and purifying gas, traditional acheson furnace and inner bunch graphitization structure are combined together, greying or carbonizing treatment, purification process are united two into one, and resulting product purity is higher, has reduced preparation cost.
The processing parameter of embodiment 1～6 and Comparative Examples is asked for an interview table 1.
As shown in Figure 3, the carbon nanotube CNT that embodiment 1 processed through the graphitization processing method, the surface topography homogeneous, through composition test, carbon content is high, and iron level is low.
The product that method of the present invention prepares, ash content is tested according to " 4.3 " the determination of ash method in the GB/T3521-2008 graphite chemical analysis method; The KYKY2800B sem observation pattern that section's tech Technology Dev Company Ltd. produces in the employing; Adopt PW3040/60X x ray diffractometer x test layer spacing and the Lc (002) of Dutch PANalytical X ' Pert, and with 30% Si (analytical pure) as interior mark; Adopt the real density of true density instrument test material; Adopt the U.S. OPTIMA of Perkinelmer Inc. 2100 DV inductive coupling plasma emission spectrographs test iron level and magnetic substance content; Adopt the PHS-3C type acidometer of Shanghai thunder magnetic instrument plant to carry out the test of pH value.
The test result of embodiment 1～6 and Comparative Examples is asked for an interview table 2.
The processing parameter of table 1 embodiment 1～6 and Comparative Examples
The test result of table 2 embodiment 1～6 and Comparative Examples
Claims (15)
1. the purifying of a graphite material and method for graphitizing may further comprise the steps: the plumbago crucible of one, carbon product being put into body of heater; Two, the speed with 100 ℃/min heats up, and the temperature of plumbago crucible reaches 1300 ℃ in stove, with 1m
3The flow of/h passes into nitrogen; Three, the speed with 100 ℃/min continues to heat up, and when temperature reaches 1600 ℃, changes into 3m
3The flow of/h passes into chlorine; Four, continue to be warming up to 2100 ℃ with the speed of 100 ℃/min, simultaneously with 1m
3The flow of/h passes into bromine gas, until temperature stopped heating when rising to 2400 ℃ changes with 5m again
3The flow of/h passes into chlorine and is reduced to below 2000 ℃ to temperature, again with 4.8m
3The flow of/h is sent into nitrogen, keeps 3h, obtains the graphite product behind the purifying.
2. the purifying of graphite material according to claim 1 and method for graphitizing is characterized in that: behind the described maintenance 3h, naturally cool to below 100 ℃.
3. the purifying of graphite material according to claim 2 and method for graphitizing is characterized in that: to the screening of the graphite product behind the purifying, except magnetic.
4. the purifying of graphite material according to claim 3 and method for graphitizing, it is characterized in that: described carbon product be fixed carbon content at the natural graphite powder more than 85%, graphous graphite powder, microlite ink powder, coking coal, coke, Graphite Electrodes, fixed carbon content more than 85%, carbon nanotube, carbon fiber or refinery coke.
5. the purifying of graphite material according to claim 4 and method for graphitizing, it is characterized in that: described plumbago crucible (4) is 30 to 90 serial connections, and each plumbago crucible (4) capacity is 50 to 300 liters.
6. the purifying of graphite material according to claim 5 and method for graphitizing is characterized in that: connect the distribution of current plate (3) of graphite matter between the stove end electrode (2) at described body of heater two ends, connect plumbago crucible (4) between the distribution of current plate (3).
7. the purifying of graphite material according to claim 6 and method for graphitizing is characterized in that: described plumbago crucible (4) is by pad (5) serial connection, and pad (5) is coated be used to the contact cream that improves the end face electrical contact performance.
8. the purifying of graphite material according to claim 7 and method for graphitizing is characterized in that: the used logical electrically heated transformer capacity of described body of heater is for being not less than 1.6 ten thousand KVA, and voltage adjusting range is at 15V to 300V.
9. the purifying of graphite material according to claim 8 and method for graphitizing, it is characterized in that: be filled with the thick metallurgical coke of 300～1000mm or refinery coke (9) insulation material between described plumbago crucible (4) and the body of heater, body of heater is made of the furnace wall (6) on furnace bottom (8) and the furnace bottom (8), bottom of furnace body pack into 200～1000mm thick metallurgical coke or refinery coke (9) furnace burdening, metallurgical coke or refinery coke (9) granularity is to 50mm greater than 0.
10. the purifying of graphite material according to claim 9 and method for graphitizing, it is characterized in that: described furnace bottom (8) is provided with ventilation carbon tube (7), one termination of ventilation carbon tube (7) enters in the body of heater, the other end connects chlorine pot (10), fluoro-gas tank (11), nitrogen pot (12), argon tanks (13) and bromine gas tank (14) through a collecting pipe, described chlorine pot (10), fluoro-gas tank (11), nitrogen pot (12), argon tanks (13) and bromine gas tank (14) are provided with valve and under meter, and collecting pipe is five to advance a connecting tube that outes.
11. the purifying of a graphite material and method for graphitizing may further comprise the steps: the plumbago crucible of one, carbon product being put into body of heater; Two, the speed with 300 ℃/min heats up, and the temperature of plumbago crucible reaches 1600 ℃ in stove, with 5m
3The flow of/h passes into argon gas; Three, the speed with 150 ℃/min continues to heat up, and when temperature reaches 1950 ℃, changes into 3.7m
3The flow of/h passes into chlorine; Four, continue to be warming up to 2050 ℃ with the speed of 5 ℃/min, simultaneously with 4m
3The flow of/h passes into freonll-11, until temperature stopped heating when rising to 2600 ℃ changes with 4.5m again
3The flow of/h passes into chlorine and is reduced to below 2000 ℃ to temperature, again with 0.1m
3The flow of/h is sent into argon gas, keeps 15h, obtains the graphite product behind the purifying.
12. the purifying of a graphite material and method for graphitizing may further comprise the steps: the plumbago crucible of one, carbon product being put into body of heater; Two, the speed with 50 ℃/min heats up, and the temperature of plumbago crucible reaches 900 ℃ in stove, with 3m
3The flow of/h passes into nitrogen; Three, the speed with 80 ℃/min continues to heat up, and when temperature reaches 1000 ℃, changes into 4.3m
3The flow of/h passes into chlorine; Four, continue to be warming up to 1400 ℃ with the speed of 80 ℃/min, simultaneously with 1m
3The flow of/h passes into freon, until temperature stopped heating when rising to 1800 ℃ changes with 3.6m again
3The flow of/h passes into chlorine and is reduced to below 1200 ℃ to temperature, again with 5m
3The flow of/h is sent into argon gas, keeps 2h, obtains the graphite product behind the purifying.
13. the purifying of a graphite material and method for graphitizing may further comprise the steps: the plumbago crucible of one, carbon product being put into body of heater; Two, the speed with 5 ℃/min heats up, and the temperature of plumbago crucible reaches 1000 ℃ in stove, with 1.2m
3The flow of/h passes into nitrogen; Three, the speed with 5 ℃/min continues to heat up, and when temperature reaches 1550 ℃, changes into 5m
3The flow of/h passes into chlorine; Four, continue to be warming up to 2050 ℃ with the speed of 120 ℃/min, simultaneously with 5m
3The flow of/h passes into bromine gas, until temperature stopped heating when rising to 2800 ℃ changes with 1.3m again
3The flow of/h passes into chlorine and is reduced to below 1000 ℃ to temperature, again with 1.0m
3The flow of/h is sent into argon gas, keeps 1h, obtains the graphite product behind the purifying.
14. the purifying of a graphite material and method for graphitizing may further comprise the steps: the plumbago crucible of one, carbon product being put into body of heater; Two, the speed with 130 ℃/min heats up, and the temperature of plumbago crucible reaches 1700 ℃ in stove, with 4m
3The flow of/h passes into argon gas; Three, the speed with 300 ℃/min continues to heat up, and when temperature reaches 1850 ℃, changes into 1m
3The flow of/h passes into chlorine; Four, continue to be warming up to 2100 ℃ with the speed of 130 ℃/min, simultaneously with 1.5m
3The flow of/h passes into freonll-11, until temperature stopped heating when rising to 3000 ℃ changes with 3m again
3The flow of/h passes into chlorine and is reduced to below 1500 ℃ to temperature, again with 1.0m
3The flow of/h is sent into argon gas, keeps 4h, obtains the graphite product behind the purifying.
15. the purifying of a graphite material and method for graphitizing may further comprise the steps: the plumbago crucible of one, carbon product being put into body of heater; Two, the speed with 260 ℃/min heats up, and the temperature of plumbago crucible reaches 1650 ℃ in stove, with 2.6m
3The flow of/h passes into nitrogen; Three, the speed with 260 ℃/min continues to heat up, and when temperature reaches 1900 ℃, changes into 2.6m
3The flow of/h passes into chlorine; Four, continue to be warming up to 2300 ℃ with the speed of 300 ℃/min, simultaneously with 2.6m
3The flow of/h passes into freon, until temperature stopped heating when rising to 3300 ℃ changes with 1m again
3The flow of/h passes into chlorine and is reduced to below 2000 ℃ to temperature, again with 2.4m
3The flow of/h is sent into nitrogen, keeps 12h, obtains the graphite product behind the purifying.
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| CN105883787A (en) * | 2016-04-14 | 2016-08-24 | 湖北鄂信钻石科技股份有限公司 | Preparation method of carbon source for synthesis of white diamond |
| CN108483440A (en) * | 2018-06-01 | 2018-09-04 | 中钢集团新型材料（浙江）有限公司 | A kind of nuclear graphite powder purifying process |
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Application publication date: 20110720 Assignee: The auspicious New Energy Technology Co., Ltd. of mountain Erich Siebert Assignor: Shenzhen BTR New Energy Material Co., Ltd. Contract record no.: 2013990000476 Denomination of invention: Purification and graphitization method of graphite material Granted publication date: 20130320 License type: Exclusive License Record date: 20130807 |
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