CN102745681B - Method and device for purifying graphite - Google Patents
Method and device for purifying graphite Download PDFInfo
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- CN102745681B CN102745681B CN201210250373.5A CN201210250373A CN102745681B CN 102745681 B CN102745681 B CN 102745681B CN 201210250373 A CN201210250373 A CN 201210250373A CN 102745681 B CN102745681 B CN 102745681B
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Abstract
The invention belongs to the technical field of graphite purification, and particularly relates to a method and a device for high-purity purification of natural graphite. The method for purifying graphite is characterized by including the steps: 1) preparing a device for purifying graphite; 2) isolating the air; 3) generating high-temperature plasma flame flows, namely loading working gas to a working gas inlet of a plasma torch, and starting the plasma torch to enable the working gas to be connected by ionization puncture to eject high-temperature plasma flame flows from the plasma torch; and 4) using the high-temperature plasma flame flows to purify graphite, namely turning on a flash valve, feeding gas into a gas injection pipe, enabling graphite raw materials to fall into the bottom of a furnace via the high-temperature plasma flame flows to obtain purified graphite, and opening a taking port to take out the purified graphite after the furnace is cooled, wherein a gas inlet valve on the gas injection pipe is in linkage with the flash valve. The method is low in energy consumption, the graphite obtained by the method is high in purity, and the device is simple.
Description
Technical field
The invention belongs to graphite purification technical field, be specifically related to a kind of method and device that natural graphite is carried out to high purity purification.
Background technology
Graphite is a kind of carbon material of highly crystalline, because of features such as its unique two-dirnentional structure and conduction, heat conduction, lubricated, high temperature resistant, stable chemical performance, make it be widely used in the fields such as metallurgy, machinery, chemical industry, fire-resistant, electronics, military project, aerospace and nuclear energy, become modern industry and height, the requisite non-metallic material of new, sharp technical development.
Along with the development of technology, the flakey high-carbon graphite product obtaining by ore-dressing technique can not meet the requirement of some high-new industry, therefore needs further to improve the purity of graphite.At present, purify the both at home and abroad method of graphite mainly contains flotation process, acid-base method, hydrofluoric acid method, chlorinating roasting, pyroprocess etc.Wherein, acid-base method, hydrofluoric acid method and chlorinating roasting belong to chemical purification method, and high temperature purification is owned by France in physical purification method.
Flotation process is to utilize the flotability of graphite to carry out enrichment purification to graphite, is mainly adapted to the natural flaky graphite that flotability is good, and graphite raw ore final concentrate grade after flotation is generally 90% left and right, sometimes can reach 94%～95%.But use this method purification graphite can only make the grade of graphite obtain limited raising, because the compounds such as part silicate minerals and potassium, sodium, calcium, magnesium, aluminium are superfine granular dip-dye in graphite scale, even if fine grinding is monomer dissociation completely, so adopt beneficiation method to be difficult to thoroughly remove this part impurity.
Acid-base method is most widely used method in high purity graphite producer of current China, its principle is that NaOH is mixed and calcined according to certain ratio with graphite, impurity under the high temperature of 500 ~ 700 DEG C in graphite is as composition and sodium hydroxide generation chemical reactions such as silicate, silico-aluminate, quartz, the water glass or the acid soluble sodium silicoaluminate that generate solubility, then wash the object that is removed to reach desiliconization with water; Another part impurity is as oxide compound of metal etc., after alkali fusion, be still retained in graphite, by the product Ore Leaching after desiliconization, make metal oxide wherein be converted into the metal-salt of solubility, and the impurity such as carbonate in graphite and alkali enter liquid phase after soaking the acid-soluble compound that forms in process and acid-respons, again by filtering, washing realizes and the separating of graphite, thereby reach the object of purification.But the shortcoming of this kind of method of purification is to need high-temperature calcination, and equipment corrosion is serious, graphite number of dropouts is large and contaminated wastewater is serious, and is difficult to production carbon content 99.9% and above high purity graphite.
Hydrofluoric acid method of purification is to utilize hydrofluoric acid to react with impurity nearly all in graphite to generate water-soluble compound and volatile matter, and then water rinses and removes impurity compound, thereby reaches the object of purification.Use hydrofluoric acid method purification graphite, dust removal rate is high, energy consumption is low, and the graphite of purification gained is of high grade, little to the performance impact of graphite.But because hydrofluoric acid has severe toxicity and severe corrosive, in production process, must there is strict safety prevention measure, strictly cause cost to raise for equipment requirements; Hydrofluoric acid method produces in addition wastewater toxicity and corrodibility are all very strong, need could discharge after strict processing, and the input of environmental protection link makes again the cost of hydrofluoric acid method greatly increase, as slightly not in place in sewage disposal, can cause huge pollution to environment.
Chlorinating roasting is by graphite ore roasting under certain high temperature and specific atmosphere, pass into again chlorine and carry out chemical reaction, make the impurity in graphite carry out chlorination reaction, the gas phase that the molten boiling point of generation is lower or the muriate of condensation product and complex compound are overflowed, thereby reach the object of purification.Due to factors such as toxicity, heavy corrosion and the contaminate environment of chlorine, limit to a certain extent applying of chlorizing calcination process.
Pyroprocess purification graphite, is one of material because of graphite is occurring in nature fusing point, boiling point is the highest, and fusing point is 3850 ± 50 DEG C, and boiling point is 4500 DEG C, far above the molten boiling point of impurities, and its this characteristic theoretical basis of pyroprocess purification graphite just.Directly pack Graphite Powder 99 into plumbago crucible, in the purifying furnace that passes into inert protective gas and a small amount of Freon gas, be heated to 2300～3000 DEG C, keep for some time, the impurity in graphite overflows because of gasification, thereby realizes the purification of graphite.Although pyroprocess can be produced more than 99.99% ultra-pure graphite, but because of calcining temperature high, must specialized designs build High Temperature Furnaces Heating Apparatus, apparatus expensive, invest huge, electric-heating technology is required strict, need isolated air, otherwise that graphite just starts be warmed up to 450 DEG C in warm air time is oxidized, temperature is higher, and the loss of graphite is just larger.In addition, the thermo-efficiency of this equipment is not high, and power consumption is very big, and the high range of application of this method that also makes of the electricity charge is very limited, only has the special industry very high to graphite specification of quality (as national defence, space flight etc.) just to adopt pyroprocess small serial production high purity graphite.
Summary of the invention
The method and the device thereof that the object of the present invention is to provide a kind of graphite of purifying, the method energy consumption is low, and the purity of the graphite obtaining is high, and its device is simple.
For achieving the above object, the technical solution used in the present invention is: a kind of method of the graphite of purifying, is characterized in that it comprises the steps:
1) preparation of the device of purification graphite;
2) isolated air: close the intake valve, exhaust port and the protection gas inlet mouth that flash on valve, gas ejector pipe, in hopper, pack graphite raw material into (in order to improve purification efficiency, the general graphite concentrate of carbon mass content >=90% of using is as raw material), vacuum pump is connected to and vacuumizes Link Port place, start vacuum pump by the state that is evacuated in body of heater (vacuum tightness is 0.01～0.05MPa), after vacuumizing, toward the logical shielding gas of protection gas inlet mouth, make body of heater internal pressure return to barometric point, after close protection gas inlet mouth;
3) produce high-temperature plasma flame stream: the work gas inlet mouth to plasma torch loads working gas, plasma torch igniting, working gas is ionized and punctures conducting, ejects high-temperature plasma flame stream from plasma torch, and temperature is up to 4000～8500 DEG C;
4) utilize high-temperature plasma flame stream purification graphite: open and flash valve, and pass into the gas with certain pressure to gas ejector pipe pulsed, intake valve on gas ejector pipe links with flashing valve, and in the time flashing valve unlatching, intake valve is opened simultaneously, and while flashing valve closure, intake valve cuts out; Graphite raw material falls by high-temperature plasma flame and flows, and falls into the bottom of body of heater, obtains the graphite after purifying; After body of heater is cooling, open material taking mouth and take out the graphite of purifying.
Described step 2) in the shielding gas that adds can be the one in argon gas, nitrogen; be preferably nitrogen; need sneak into a certain amount of Freon gas for improving purification efficiency; the volume content of Freon gas is between 0.05%～0.5%; also be that shielding gas can be argon gas and Freon gas, or nitrogen and Freon gas.
The working gas passing in described step 3) is argon gas or nitrogen, is preferably nitrogen.
The gas with certain pressure passing in described step 4) is argon gas or nitrogen, is preferably nitrogen; Gaseous tension is 0.8MPa～2.5MPa.
In order to obtain more highly purified graphite, the graphite after purifying is come back in hopper and is again entered in body of heater, repeatedly repeating step 2)～4) repeatedly purify, described is repeatedly 1～20 time.
Realize a device for the purification graphite of aforesaid method, it is characterized in that it comprises body of heater, hopper, plasma torch; Hopper is fixedly mounted on the top of body of heater, and the discharge port of hopper communicates with the cavity in body of heater, is provided with and flashes valve at the discharge port place of hopper, flashes the cavity that valve is fixed on body of heater, is positioned at body of heater; The upper end of body of heater is provided with gas ejector pipe and exhaust port, and exhaust port is positioned at the below of gas ejector pipe; The bottom of body of heater is provided with protection gas inlet mouth and the Link Port that vacuumizes for being connected with vacuum pump, and vacuumizes Link Port and is positioned at the below of protecting gas inlet mouth, is provided with sealable material taking mouth in the bottom of body of heater; Plasma torch is laterally disposed on body of heater, and the spout of plasma torch communicates with the cavity of body of heater, and the upper end of plasma torch is provided with work gas inlet mouth.
The Double-layer vertical hollow circuit cylinder body structure that described body of heater is made up of liner and shell, shell adopts stainless steel to be made, and liner is that one deck is attached to the graphite brick on outer casing inner wall.
Described plasma torch connects housing and power cabinet successively by cable, supply with power by power cabinet to plasma torch, the temperature flowing by the flame of the parameters such as housing control working gas flow, pressure, electric current, voltage and then the ejection of adjusting plasma torch.
One end of described gas ejector pipe extends to the inside of body of heater, and one end of gas ejector pipe is socketed with blast cap, and blast cap is positioned at the below of flashing valve.This blast cap plays cloth wind action, graphite raw material can be dispelled from the pulsed high pressure draft of blast cap ejection, is more conducive to the purifying of graphite.
On described body of heater, extend one section of body of heater extension consistent with plasma torch angle of inclination, the central axis of body of heater extension and the central axis of plasma torch are same axis, this body of heater extension is positioned at the opposite side of the body of heater relative with plasma torch, and the bottom of body of heater extension is interconnected by passage and body of heater.When graphite raw material is scattered while flowing by plasma flame from hopper, the air-flow of plasma flame stream can be brought into a part of graphite in body of heater extension, then falls into the bottom of body of heater along passage.
Compared with prior art, the invention has the beneficial effects as follows: new technology, device are simply, energy consumption is low, intensification is rapid, it is using plasma torch heating technique, utilize thermal plasma part to exceed the high temperature of 4000 DEG C, make the impurity fully gasification at short notice in graphite raw material, thereby realize the object of purification graphite, can also realize the continuous purification of graphite.Principle of the present invention is consistent with existing high temperature purification method, but owing to being that Graphite Powder 99 is directly sent into direct heating in the plasma flame stream with excessive temperature, therefore heat utilization efficiency is high.And adopting existing High Temperature Furnaces Heating Apparatus to purify, heat energy is more at heating furnace body except adding thermal material, and is dispersed in environment.Therefore energy consumption of the present invention is far below existing high temperature purification method.
The purity high (carbon mass content >=98.7%) of the graphite obtaining.Initial carbon mass content 90%, granularity 100 object graphite, carbon mass content 98.7% after primary purification; Through the carbon mass content 99.5% of purifying for the second time; Through the carbon mass content 99.9% of purifying for the third time; As again through the graphite purification that circulates several times to carbon mass content 99.99%.
Brief description of the drawings
Fig. 1 is the purify structural representation of device of graphite of the present invention.
In figure: 1-body of heater; 11-liner; 12-shell; 13-gas ejector pipe; 14-exhaust port; 15-protection gas inlet mouth; 16-vacuumizes Link Port; 17-material taking mouth; 2-hopper; 3-flashes valve; 4-blast cap; 5-plasma torch; 51-work gas inlet mouth; 6-housing; 7-power cabinet; 8-body of heater extension; 81-passage.
Embodiment
In order to understand better the present invention, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention is not only confined to the following examples.
Embodiment 1, consults shown in Fig. 1,
The purify method of graphite, it comprises the steps:
1) preparation of the device of purification graphite;
2) isolated air: close the intake valve, exhaust port 14 and the protection gas inlet mouth 15 that flash on valve 3, gas ejector pipe 13, in hopper 2, pack graphite raw material into (in order to improve purification efficiency, the general graphite concentrate of carbon mass content >=90% of using is as raw material), vacuum pump is connected to and vacuumizes Link Port 16 places, start vacuum pump by the state that is evacuated in body of heater 1 (vacuum tightness is 0.01～0.05MPa), after vacuumizing, toward protection gas inlet mouth 15 logical shielding gas, make body of heater 1 internal pressure return to barometric point, after close protection gas inlet mouth 15; In order to ensure the nonoxidizing atmosphere in stove, can repeatedly vacuumize---fill shielding gas;
3) produce high-temperature plasma flame stream: the work gas inlet mouth 51 to plasma torch 5 loads working gas, power-on cabinet 7 is lighted a fire plasma torch 5, working gas is ionized and punctures conducting, from plasma torch 5, eject high-temperature plasma flame stream, high temperature is up to 4000～8500 DEG C;
4) utilize high-temperature plasma flame stream purification graphite: open and flash valve 3, and pass into the gas with certain pressure to gas ejector pipe 13 pulseds, intake valve on gas ejector pipe 13 with flash valve 3 and link, in the time flashing valve 3 and open, intake valve is opened simultaneously, while flashing valve 3 closure, intake valve cuts out, thereby reach, the graphite raw material falling in hopper 2 is dispelled to the effect that is the shape that seethes with excitement; Graphite raw material falls by high-temperature plasma flame and flows, in the process that falls to flowing by high-temperature plasma flame at the graphite raw material scattering, graphite and wherein impurity are warmed to excessive temperature by moment, impurity in raw material is vaporized and is converted into volatile matter, this volatile matter is under the effect of pyroreaction air pressure, discharge out of the furnace by exhaust port 14, after purification system is processed, enter atmosphere, and fall into the graphite after high temperature purification that is of body of heater 1 bottom; After body of heater 1 is cooling, open material taking mouth 17 and take out the graphite of purifying.
Described step 2) in the shielding gas that adds can be the one in argon gas, nitrogen; be preferably nitrogen; need sneak into a certain amount of Freon gas for improving purification efficiency; the volume content of Freon gas is between 0.05%～0.5%; also be that shielding gas can be argon gas and Freon gas, or nitrogen and Freon gas.
The working gas passing in described step 3) is argon gas or nitrogen, is preferably nitrogen.
The gas with certain pressure passing in described step 4) is argon gas or nitrogen, is preferably nitrogen; Gaseous tension is 0.8MPa～2.5MPa.
Initial carbon mass content 90%, granularity 100 object graphite, carbon mass content 98.7% after primary purification.
The device of above-mentioned a kind of purification graphite of realizing aforesaid method, it comprises body of heater 1, hopper 2, plasma torch 5; Hopper 2 is fixedly mounted on the top of body of heater 1, and the discharge port of hopper 2 communicates with the cavity in body of heater 1, is provided with and flashes valve 3 at the discharge port place of hopper 2, flashes the cavity that valve 3 is fixed on body of heater 1, is positioned at body of heater 1; The upper end of body of heater 1 is provided with gas ejector pipe 13 and exhaust port 14, and exhaust port 14 is positioned at the below of gas ejector pipe 13; The bottom of body of heater 1 is provided with protection gas inlet mouth 15 and vacuumizes Link Port 16 with for what be connected with vacuum pump, vacuumize the below that Link Port 16 is positioned at protection gas inlet mouth 15, be provided with sealable material taking mouth 17 in the bottom of body of heater 1, for taking out the material after purification; Plasma torch 5 is laterally disposed on body of heater 1, and the spout of plasma torch 5 communicates with the cavity of body of heater 1, and the upper end of plasma torch 5 is provided with work gas inlet mouth 51.
The Double-layer vertical hollow circuit cylinder body structure that described body of heater 1 is made up of liner 11 and shell 12, shell 12 adopts stainless steel to be made, and liner 11 is attached to the graphite brick on shell 12 inwalls for one deck.
Described plasma torch 5 connects housing 6 and power cabinet 7 successively by cable, supply with power by power cabinet 7 to plasma torch 5, control the parameters such as working gas flow, pressure, electric current, voltage by housing 6 and then regulate the temperature of the flame stream that plasma torch 5 sprays.
One end of described gas ejector pipe 13 extends to the inside (in cavity) of body of heater 1, and one end of gas ejector pipe 13 is socketed with blast cap 4, and blast cap 4 is positioned at the below of flashing valve 3.Blast cap 4 plays cloth wind action, and the pulsed high pressure draft spraying from blast cap 4 can dispel graphite raw material, is more conducive to the purifying of graphite.
On described body of heater 1, extend one section of body of heater extension 8 consistent with plasma torch 5 angles of inclination, the central axis of the central axis of body of heater extension 8 and plasma torch 5 is same axis, this body of heater extension 8 is positioned at the opposite side of the body of heater relative with plasma torch 51, that is: plasma torch 5 is positioned at a side of body of heater 1, and this body of heater extension 8 is positioned at the opposite side of body of heater 1.The bottom of body of heater extension 8 is interconnected by passage 81 and body of heater 1, when graphite raw material is scattered while flowing by plasma flame from hopper 2, the air-flow of plasma flame stream can be brought into a part of graphite in body of heater extension 8, then falls into the bottom of body of heater 1 along passage 81.
Embodiment 2,
Substantially the same manner as Example 1, difference is: in order to obtain more highly purified graphite, repeating step 2)～4) carry out primary purification [graphite after purifying is come back in hopper 2 and again entered in body of heater 1, through purifying for the second time].Initial carbon mass content 90%, granularity 100 object graphite, carbon mass content 98.7% after primary purification; Through the carbon mass content 99.5% of purifying for the second time.
Embodiment 3,
Substantially the same manner as Example 1, difference is: in order to obtain more highly purified graphite, repeating step 2)～4) carry out secondary purification [graphite after purifying is come back in hopper 2 and again entered in body of heater 1, through purifying for the third time].Initial carbon mass content 90%, granularity 100 object graphite, carbon mass content 98.7% after primary purification; Through the carbon mass content 99.5% of purifying for the second time; Through the carbon mass content 99.9% of purifying for the third time.
Embodiment 4,
Substantially the same manner as Example 1, difference is: in order to obtain more highly purified graphite, repeating step 2)～4) carry out purifying for 20 times [graphite after purifying is come back in hopper 2 and again entered in body of heater 1, through 20 circulation graphite purifications].Initial carbon mass content 90%, granularity 100 object graphite, through 20 circulation graphite purifications to carbon mass content 99.99%.
Claims (10)
1. the purify method of graphite, is characterized in that it comprises the steps:
1) preparation of the device of purification graphite;
2) isolated air: close the intake valve, exhaust port (14) and the protection gas inlet mouth (15) that flash on valve (3), gas ejector pipe (13), in hopper (2), pack graphite raw material into, vacuum pump is connected to and vacuumizes Link Port (16) and locate, start vacuum pump by the state that is evacuated in body of heater (1), after vacuumizing, toward the logical shielding gas of protection gas inlet mouth (15), make body of heater (1) internal pressure return to barometric point, after close protection gas inlet mouth (15);
3) produce high-temperature plasma flame stream: the work gas inlet mouth (51) to plasma torch (5) loads working gas, plasma torch (5) igniting, working gas is ionized and punctures conducting, ejects high-temperature plasma flame stream from plasma torch (5);
4) utilize high-temperature plasma flame stream purification graphite: open and flash valve (3), and pass into gas to gas ejector pipe (13), the intake valve on gas ejector pipe (13) with flash valve (3) interlock; Graphite raw material falls by high-temperature plasma flame and flows, and falls into the bottom of body of heater (1), obtains the graphite after purifying; After body of heater (1) is cooling, open material taking mouth (17) and take out the graphite of purifying.
2. the method for a kind of graphite of purifying according to claim 1, is characterized in that, described step 2) in the shielding gas that adds be the one in argon gas, nitrogen; Or argon gas and Freon gas, or nitrogen and Freon gas, wherein the volume content of Freon gas is 0.05%～0.5%.
3. the method for a kind of graphite of purifying according to claim 1, is characterized in that, the working gas passing in described step 3) is argon gas or nitrogen.
4. the method for a kind of graphite of purifying according to claim 1, is characterized in that, in described step 4), passing into gas is argon gas or nitrogen, and gaseous tension is 0.8MPa～2.5MPa.
5. the method for a kind of graphite of purifying according to claim 1, is characterized in that, the graphite after step 4) is purified comes back in hopper (2) and again enters in body of heater (1), repeating step 2)～4) repeatedly purify.
6. realize in claim 1-5 a device for the purification graphite of method described in arbitrary claim, it is characterized in that it comprises body of heater (1), hopper (2), plasma torch (5); Hopper (2) is fixedly mounted on the top of body of heater (1), and the discharge port of hopper (2) communicates with the cavity in body of heater (1), is provided with and flashes valve (3) at the discharge port place of hopper (2); The upper end of body of heater (1) is provided with gas ejector pipe (13) and exhaust port (14), and exhaust port (14) is positioned at the below of gas ejector pipe (13); The bottom of body of heater (1) is provided with protection gas inlet mouth (15) and vacuumizes Link Port (16) with for what be connected with vacuum pump, vacuumize the below that Link Port (16) is positioned at protection gas inlet mouth (15), be provided with sealable material taking mouth (17) in the bottom of body of heater (1); Plasma torch (5) is laterally disposed upper at body of heater (1), and the spout of plasma torch (5) communicates with the cavity of body of heater (1), and the upper end of plasma torch (5) is provided with work gas inlet mouth (51).
7. the device of purification graphite according to claim 6, it is characterized in that, the Double-layer vertical hollow circuit cylinder body structure that described body of heater (1) is made up of liner (11) and shell (12), shell (12) adopts stainless steel to be made, and liner (11) is attached to the graphite brick on shell (12) inwall for one deck.
8. the device of purification graphite according to claim 6, is characterized in that, described plasma torch (5) connects housing (6) and power cabinet (7) successively by cable.
9. the device of purification graphite according to claim 6, is characterized in that, one end of described gas ejector pipe (13) extends to the inside of body of heater (1), and one end of gas ejector pipe (13) is socketed with blast cap (4), and blast cap (4) is positioned at the below of flashing valve (3).
10. the device of purification graphite according to claim 6, it is characterized in that, on described body of heater (1), extend one section of body of heater extension (8) consistent with plasma torch (5) angle of inclination, body of heater extension (8) is positioned at the opposite side of the body of heater (1) relative with plasma torch (5), and the bottom of this body of heater extension (8) is interconnected by passage (81) and body of heater (1).
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