CN111792641A - Graphite purification method - Google Patents
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- CN111792641A CN111792641A CN202010696317.9A CN202010696317A CN111792641A CN 111792641 A CN111792641 A CN 111792641A CN 202010696317 A CN202010696317 A CN 202010696317A CN 111792641 A CN111792641 A CN 111792641A
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Abstract
A graphite purification method relates to a graphite purification method, and belongs to the technical field of graphite purification. The invention aims to solve the technical problems that the prior method purifies graphite to the purity of more than 99.99 percent, has high energy consumption, reduces the reaction efficiency of reaction components and impurities in a continuous gas passing mode, and causes the waste of a large amount of atmosphere and the increase of cost and environmental protection pressure. The method comprises the following steps: heating to 800-1000 ℃ under the absolute vacuum degree of 10-100 pa, and then introducing carbon tetrachloride under the condition of heat preservation; heating to 1200-1450 ℃, preserving heat, and alternately introducing carbon tetrachloride and argon; heating to 1600-1800 ℃, preserving heat, and alternately introducing carbon tetrachloride and argon; the method can reduce the consumption of graphite purification devices and energy sources by the conventional high-temperature method, reduce the graphite purification temperature to be less than 2000 ℃ and less than 1800 ℃, effectively improve the utilization rate of carbon tetrachloride and the discharge efficiency of impurity volatile matters by alternately introducing and exhausting, and has the advantages of simple process, high production efficiency, environmental protection and energy conservation.
Description
Technical Field
The invention relates to a graphite purification method, and belongs to the technical field of graphite purification.
Background
The graphite has the advantages of low density, corrosion resistance, radiation resistance, self-lubrication, high and low temperature resistance and the like, and has important application value in the fields of aerospace, war industry, electronics, nuclear energy, metallurgy and the like. With the rapid development of modern science and technology, the purity of graphite materials in various industrial fields has higher requirements, the use characteristics and the comprehensive performance of the graphite materials are determined by the purity of the graphite, and the higher the purity of the graphite is, the higher the application value is. The high-purity graphite refers to graphite with fixed carbon content of more than 99.9%, and the production of the high-purity graphite mainly removes impurities in the graphite through a purification process. The main impurity components contained in graphite are oxides of potassium, sodium, magnesium, iron, calcium, aluminum and the like and silicate minerals, and the conventional methods for producing high-purity graphite at home and abroad generally comprise a chemical method (hydrofluoric acid method and chlorination roasting method) and a physical method (high-temperature method). The hydrofluoric acid method is to utilize impurity in graphite and hydrofluoric acid to react and produce fluoride and volatile matter dissolved in water and achieve the goal of purifying, said method is corrosive to apparatus, and the toxicity is strong; the chloridizing roasting method is to convert impurities in the graphite into volatile matters by adopting chlorine gas, the chlorine gas has strong corrosivity and toxicity, the purchasing and transportation cost is higher, the environment is polluted, the process system is unstable, the production cost is high, and the popularization and the application of the process are limited to a certain extent; the high-temperature method mainly comprises the step of continuously heating medium-carbon or high-carbon graphite at a higher process temperature to volatilize impurities in the graphite above a boiling point so as to achieve the purpose of purification. However, the high-purity graphite prepared by the high-temperature method has the following problems: firstly, medium carbon or high carbon graphite is purified to the purity of more than 99.99 percent, high temperature furnace equipment needs to continuously work for more than 5 hours at the high temperature of about 3000 ℃, higher requirements are put forward on the performance of the equipment, the energy consumption is higher, secondly, a large amount of impurity volatile matters are generated in the purification process, the requirements on the pollution resistance and the corrosion resistance of the equipment are high, and in the purification process, gas continuously passes through the purification process, so that the reaction efficiency of reaction components and impurities is reduced, and simultaneously, a large amount of atmosphere waste and the increase of the cost and the environmental protection pressure are caused.
Disclosure of Invention
The invention aims to solve the technical problems that the prior method purifies graphite to the purity of more than 99.99 percent, has high energy consumption, reduces the reaction efficiency of reaction components and impurities in a continuous gas passing mode, simultaneously causes the waste of a large amount of atmosphere and increases the cost and the environmental protection pressure, and provides a graphite purification method.
The graphite purification method comprises the following steps:
firstly, laying medium-carbon graphite or high-carbon graphite in a graphite crucible, then moving the graphite crucible into a high-temperature purification furnace, sealing the furnace body, and starting a vacuum pumping system until the absolute vacuum degree reaches 10 pa-100 pa;
secondly, heating to 800-1000 ℃, then preserving heat for 0.5-1 h, and introducing carbon tetrachloride at the flow rate of 0.5-1.5L/h while preserving heat;
thirdly, heating to 1200-1450 ℃, then preserving heat for 1-1.5 h, alternately introducing carbon tetrachloride and argon with the purity of 99.999% into the furnace while preserving heat, wherein the flow rate of introducing the carbon tetrachloride is 0.5L-1.5L/h, and the flow rate of introducing the high-purity argon is 2-3 m3/h；
The mode of alternately introducing carbon tetrachloride and argon with the purity of 99.999 percent into the furnace is as follows: after carbon tetrachloride is introduced for 10-15 min, closing an air inlet of the carbon tetrachloride, opening an argon inlet after 20-30 min, simultaneously opening an exhaust port, closing the exhaust port and the argon inlet after 30min, and repeatedly introducing carbon tetrachloride;
fourthly, heating to 1600-1800 ℃, then preserving heat for 1.5-2 h, alternately introducing carbon tetrachloride and argon with the purity of 99.999 percent into the furnace while preserving heat, wherein the flow rate of introducing the carbon tetrachloride is 0.5L-1.5L/h, and the flow rate of introducing the high-purity argon is 2-3 m3H, obtaining high-purity graphite;
the mode of alternately introducing carbon tetrachloride and argon with the purity of 99.999 percent into the furnace is as follows: and (3) after carbon tetrachloride is introduced for 10-15 min, closing an air inlet of the carbon tetrachloride, opening an argon inlet after 20-30 min, simultaneously opening an exhaust port, closing the exhaust port and the argon inlet after 30min, and repeatedly introducing carbon tetrachloride.
The heating rate in the first step, the second step and the third step is 15 ℃/min.
The purification raw material can be medium-carbon graphite or high-carbon graphite, wherein the purity of the medium-carbon graphite is 80-93%, and the purity of the high-carbon graphite is 94-98%. After the medium carbon graphite with lower purity is purified, the fixed carbon content can be improved to more than 99.99 percent.
The flow rate of the introduced carbon tetrachloride is related to the purity level of the raw materials, and the introduced argon with the purity of 99.999 percent is mainly used for protecting the furnace chamber and simultaneously can intermittently discharge the impurity atmosphere generated in the furnace; and step four, after the purification is finished, the atmosphere in the furnace is replaced by inert gas, so that residual impurity volatile matters can be removed, and the high-temperature oxidation of the purified graphite is prevented. The flow rates described in the present invention are based on the furnace volume per cubic meter.
Compared with the purification effect of graphite raw materials with different particle sizes of 100-500 mu m, the content of fixed carbon after purification can reach more than 99.99 percent.
The invention has the beneficial effects that:
1. the intermittent alternate ventilation and exhaust mode adopted by the invention effectively improves the reaction efficiency and the utilization rate of the reaction gas, and has obvious emission reduction effect;
2. the heat preservation at different specific temperatures for a plurality of time periods involved in the process steps of the invention is designed for different boiling points of different impurities in graphite. Because the content of Si in the graphite impurities is relatively high, Si and Fe are mainly removed in a chloride form in a heat preservation range of 800-1000 ℃ so as to avoid SiC generated in a high-temperature region and difficult removal; impurities such as Na, Mg and the like are mainly removed in a chloride mode in the temperature preservation range of 1200-1450 ℃; the temperature-preserving range of 1600-1800 ℃ is mainly used for removing K, Ca and other impurities. Therefore, the heat preservation in different temperature intervals is crucial to the purification effect of graphite, and experiments prove that the purification effect is obviously improved by adopting the method provided by the invention;
3. the purification method provided by the invention can reduce the consumption of a graphite purification device and energy sources by a conventional high-temperature method, reduce the graphite purification temperature to be less than 2000 ℃ and less than 1800 ℃, effectively improve the utilization rate of carbon tetrachloride and the discharge efficiency of impurity volatile matters by alternately introducing and exhausting, create conditions for the industrial production of high-purity graphite with the carbon content of more than 99.99%, and simultaneously have the advantages of simple process, high production efficiency, environmental protection, energy conservation and the like, and have good industrialization prospect and strong practical popularization value.
Detailed Description
The technical solution of the present invention is not limited to the following specific embodiments, but includes any combination of the specific embodiments.
The first embodiment is as follows: the graphite purification method of the present embodiment is as follows:
firstly, laying medium-carbon graphite or high-carbon graphite in a graphite crucible, then moving the graphite crucible into a high-temperature purification furnace (GJC-TCL-400 horizontal high-temperature furnace, produced by Guangchang technology Limited, Ltd., in Zhou province), sealing the furnace body, and starting a vacuum-pumping system until the absolute vacuum degree reaches 10 pa-100 pa;
secondly, heating to 800-1000 ℃, then preserving heat for 0.5-1 h, and introducing carbon tetrachloride at the flow rate of 0.5-1.5L/h while preserving heat;
thirdly, heating to 1200-1450 ℃, then preserving heat for 1-1.5 h, alternately introducing carbon tetrachloride and argon with the purity of 99.999% into the furnace while preserving heat, wherein the flow rate of introducing the carbon tetrachloride is 0.5L-1.5L/h, and the flow rate of introducing the high-purity argon is 2-3 m3/h；
The mode of alternately introducing carbon tetrachloride and argon with the purity of 99.999 percent into the furnace is as follows: after carbon tetrachloride is introduced for 10-15 min, closing an air inlet of the carbon tetrachloride, opening an argon inlet after 20-30 min, simultaneously opening an exhaust port, closing the exhaust port and the argon inlet after 30min, and repeatedly introducing carbon tetrachloride;
fourthly, heating to 1600-1800 ℃, then preserving heat for 1.5-2 h, alternately introducing carbon tetrachloride and argon with the purity of 99.999 percent into the furnace while preserving heat, wherein the flow rate of introducing the carbon tetrachloride is 0.5L-1.5L/h, and the flow rate of introducing the high-purity argon is 2-3 m3H, obtaining high-purity graphite;
the mode of alternately introducing carbon tetrachloride and argon with the purity of 99.999 percent into the furnace is as follows: and (3) after carbon tetrachloride is introduced for 10-15 min, closing an air inlet of the carbon tetrachloride, opening an argon inlet after 20-30 min, simultaneously opening an exhaust port, closing the exhaust port and the argon inlet after 30min, and repeatedly introducing carbon tetrachloride.
After the heat preservation is finished, opening the exhaust port of the furnace body to connect the exhausted gas into the waste gas absorption device, and continuing to use 3m3Introducing high-purity argon for 0.5h at a flow rate of/h until the atmosphere in the furnace is replaced by inert gas and micro-positive pressure is maintained, and closing all gas inlets and outlets.
The second embodiment is as follows: the difference between the present embodiment and the first embodiment is that the temperature rise rate in the first step, the second step and the third step is 15 ℃/min. The rest is the same as the first embodiment.
The third concrete implementation mode: the difference between the embodiment and the first or second embodiment is that the temperature is increased to 800 ℃ in the second step, then the temperature is preserved for 0.5h, and carbon tetrachloride is introduced at the flow rate of 0.5L/h while the temperature is preserved. The others are the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between the embodiment and the first to the third embodiment is that in the second step, the temperature is increased to 900 ℃, then the temperature is preserved for 0.5h, and carbon tetrachloride is introduced at the flow rate of 1L/h while the temperature is preserved. The rest is the same as one of the first to third embodiments.
The fifth concrete implementation mode: the difference between the embodiment and one of the first to the fourth embodiments is that in the second step, the temperature is raised to 1000 ℃, then the temperature is preserved for 0.5h, and carbon tetrachloride is introduced at the flow rate of 1.5L/h while the temperature is preserved. The rest is the same as one of the first to fourth embodiments.
The sixth specific implementation mode: the difference between the embodiment and the first to the fifth embodiment is that the temperature is raised to 1200 ℃ in the third step, then the temperature is kept for 1h, carbon tetrachloride and argon with the purity of 99.999 percent are alternately introduced into the furnace while the temperature is kept, the flow rate of the carbon tetrachloride is 0.5L/h, and the flow rate of the high-purity argon is 2m3H is used as the reference value. The rest is the same as one of the first to fifth embodiments.
The seventh embodiment: the difference between the embodiment and the first to the sixth embodiment is that the temperature is raised to 1300 ℃ in the third step, then the temperature is kept for 1.5h, carbon tetrachloride and argon with the purity of 99.999 percent are alternately introduced into the furnace while the temperature is kept, the flow rate of the carbon tetrachloride is 1L/h, and the flow rate of the high-purity argon is 2.5m3H is used as the reference value. The rest is the same as one of the first to sixth embodiments.
The specific implementation mode is eight: the difference between the first embodiment and the seventh embodiment is that the temperature is raised to 1400 ℃ in the third step, then the temperature is kept for 1.5h, carbon tetrachloride and argon with the purity of 99.999 percent are alternately introduced into the furnace while the temperature is kept, the flow rate of the carbon tetrachloride is 1.5L/h, and the flow rate of the high-purity argon is 3m3H is used as the reference value. OthersThe same as in one of the first to seventh embodiments.
The specific implementation method nine: the difference between the embodiment and the first to eighth embodiment is that the temperature is raised to 1600 ℃ in the fourth step, then the temperature is kept for 1.5h, carbon tetrachloride and argon with the purity of 99.999 percent are alternately introduced into the furnace while the temperature is kept, the flow rate of the carbon tetrachloride is 0.5L/h, and the flow rate of the high-purity argon is 2m3H is used as the reference value. The rest is the same as the first to eighth embodiments.
The detailed implementation mode is ten: the difference between the first embodiment and the ninth embodiment is that the temperature is raised to 1700 ℃ in the fourth step, then the temperature is preserved for 1.5h, carbon tetrachloride and argon with the purity of 99.999 percent are alternately introduced into the furnace while the temperature is preserved, the flow rate of the carbon tetrachloride is 0.8L/h, and the flow rate of the high-purity argon is 2.3m3H is used as the reference value. The rest is the same as one of the first to ninth embodiments.
The following experiments are adopted to verify the effect of the invention:
experiment one:
the graphite purification method comprises the following steps:
firstly, laying medium-carbon graphite or high-carbon graphite in a graphite crucible, then moving the graphite crucible into a high-temperature purification furnace (GJC-TCL-400 horizontal high-temperature furnace, produced by Guangchang technology Limited, Ltd., in Zhou province), sealing the furnace body, and starting a vacuum-pumping system until the absolute vacuum degree reaches 50 pa;
secondly, heating to 800 ℃ at the speed of 15 ℃/min, then preserving heat for 0.5h, and introducing carbon tetrachloride at the flow rate of 0.5L/h while preserving heat;
thirdly, heating to 1200 ℃ at the speed of 15 ℃/min, then preserving heat for 1h, alternately introducing carbon tetrachloride and argon with the purity of 99.999 percent into the furnace while preserving heat, wherein the flow rate of introducing the carbon tetrachloride is 0.5L/h, and the flow rate of introducing the high-purity argon is 2m3/h；
The mode of alternately introducing carbon tetrachloride and argon with the purity of 99.999 percent into the furnace is as follows: after carbon tetrachloride is introduced for 10min, the air inlet of the carbon tetrachloride is closed, after 20min, the argon inlet is opened, the exhaust port is opened, after 30min, the exhaust port and the argon inlet are closed, and then carbon tetrachloride is introduced repeatedly;
fourthly, 15 is usedHeating to 1600 deg.C at a speed of 1600 deg.C/min, maintaining the temperature for 1.5 hr, and alternately introducing carbon tetrachloride and argon gas with a purity of 99.999% into the furnace while maintaining the temperature, wherein the flow rate of carbon tetrachloride is 0.5L/hr, and the flow rate of high-purity argon gas is 2m3H, obtaining high-purity graphite;
the mode of alternately introducing carbon tetrachloride and argon with the purity of 99.999 percent into the furnace is as follows: and (3) introducing carbon tetrachloride for 10min, closing the air inlet, opening the argon inlet after 20min, opening the exhaust port at the same time, closing the exhaust port and the argon inlet after 30min, and repeatedly introducing carbon tetrachloride.
After the heat preservation is finished, opening the exhaust port of the furnace body to connect the exhausted gas into the waste gas absorption device, and continuing to use 3m3Introducing high-purity argon for 0.5h at a flow rate of/h until the atmosphere in the furnace is replaced by inert gas and micro-positive pressure is maintained, and closing all gas inlets and outlets.
The fixed carbon content of the graphite treated by the experiment is 99.99 percent (a high-temperature oxidation method is adopted, namely, accurately weighed high-purity graphite powder is put into a platinum crucible and is roasted at high temperature in an aerobic furnace at 850-900 ℃, and the fixed carbon in the graphite is oxidized at high temperature to generate CO2And weighing the residual substances, wherein the ratio of the weight loss to the weight of the original graphite powder is the fixed carbon content of the graphite powder, and a weighing instrument adopts a one ten-thousandth electronic balance).
Experiment two:
the graphite purification method comprises the following steps:
firstly, laying medium-carbon graphite or high-carbon graphite in a graphite crucible in a layered manner, then moving the graphite crucible into a high-temperature purification furnace (GJC-TCL-400 horizontal high-temperature furnace, produced by Guangchang technology Limited, Ltd., in Shangzi), sealing the furnace body, and starting a vacuum-pumping system until the absolute vacuum degree reaches 50 pa;
secondly, heating to 900 ℃ at the speed of 15 ℃/min, then preserving heat for 0.5h, and introducing carbon tetrachloride at the flow rate of 1L/h while preserving heat;
thirdly, heating to 1300 ℃ at the speed of 15 ℃/min, then preserving heat for 1.5h, alternately introducing carbon tetrachloride and argon with the purity of 99.999 percent into the furnace while preserving heat, wherein the flow rate of introducing the carbon tetrachloride is 1L/h, and the flow rate of introducing the high-purity argon is 2.5m3/h；
The mode of alternately introducing carbon tetrachloride and argon with the purity of 99.999 percent into the furnace is as follows: after carbon tetrachloride is introduced for 12min, closing an air inlet of the carbon tetrachloride, opening an argon inlet after 23min, simultaneously opening an exhaust port, closing the exhaust port and the argon inlet after 30min, and repeatedly introducing carbon tetrachloride;
fourthly, heating to 1700 ℃ at the speed of 15 ℃/min, then preserving heat for 1.5h, alternately introducing carbon tetrachloride and argon with the purity of 99.999 percent into the furnace while preserving heat, wherein the flow rate of introducing the carbon tetrachloride is 0.8L/h, and the flow rate of introducing the high-purity argon is 2.3m3H, obtaining high-purity graphite;
the mode of alternately introducing carbon tetrachloride and argon with the purity of 99.999 percent into the furnace is as follows: and (3) after carbon tetrachloride is introduced for 15min, closing the air inlet of the carbon tetrachloride, opening the argon inlet after 25min, simultaneously opening the exhaust port, closing the exhaust port and the argon inlet after 30min, and repeatedly introducing carbon tetrachloride.
After the heat preservation is finished, opening the exhaust port of the furnace body to connect the exhausted gas into the waste gas absorption device, and continuing to use 3m3Introducing high-purity argon for 0.5h at a flow rate of/h until the atmosphere in the furnace is replaced by inert gas and micro-positive pressure is maintained, and closing all gas inlets and outlets.
The fixed carbon content of the graphite treated by the experiment is 99.999 percent (a high-temperature oxidation method is adopted, namely, accurately weighed high-purity graphite powder is put into a platinum crucible and is roasted at high temperature in an aerobic furnace at 850-900 ℃, and the fixed carbon in the graphite is oxidized at high temperature to generate CO2And weighing the residual substances, wherein the ratio of the weight loss to the weight of the original graphite powder is the fixed carbon content of the graphite powder, and a weighing instrument adopts a one ten-thousandth electronic balance).
Experiment three:
the graphite purification method comprises the following steps:
firstly, laying medium-carbon graphite or high-carbon graphite in a graphite crucible in a layered manner, then moving the graphite crucible into a high-temperature purification furnace (GJC-TCL-400 horizontal high-temperature furnace, produced by Guangchang technology Limited, Ltd., in Shangzi), sealing the furnace body, and starting a vacuum-pumping system until the absolute vacuum degree reaches 100 pa;
secondly, heating to 1000 ℃ at the speed of 15 ℃/min, then preserving heat for 0.5h, and introducing carbon tetrachloride at the flow rate of 1.5L/h while preserving heat;
thirdly, heating to 1400 ℃ at the speed of 15 ℃/min, then preserving heat for 1.5h, alternately introducing carbon tetrachloride and argon with the purity of 99.999 percent into the furnace while preserving heat, wherein the flow rate of introducing the carbon tetrachloride is 1.5L/h, and the flow rate of introducing the high-purity argon is 3m3/h；
The mode of alternately introducing carbon tetrachloride and argon with the purity of 99.999 percent into the furnace is as follows: after carbon tetrachloride is introduced for 10-15 min, closing an air inlet of the carbon tetrachloride, opening an argon inlet after 20-30 min, simultaneously opening an exhaust port, closing the exhaust port and the argon inlet after 30min, and repeatedly introducing carbon tetrachloride;
fourthly, heating to 1800 ℃ at the speed of 15 ℃/min, then preserving heat for 2 hours, alternately introducing carbon tetrachloride and argon with the purity of 99.999 percent into the furnace while preserving heat, wherein the flow rate of introducing the carbon tetrachloride is 0.7L/h, and the flow rate of introducing the high-purity argon is 2.8m3H, obtaining high-purity graphite;
the mode of alternately introducing carbon tetrachloride and argon with the purity of 99.999 percent into the furnace is as follows: and (3) after carbon tetrachloride is introduced for 15min, closing the air inlet of the carbon tetrachloride, opening the argon inlet after 30min, simultaneously opening the exhaust port, closing the exhaust port and the argon inlet after 30min, and repeatedly introducing carbon tetrachloride.
After the heat preservation is finished, opening the exhaust port of the furnace body to connect the exhausted gas into the waste gas absorption device, and continuing to use 3m3Introducing high-purity argon for 0.5h at a flow rate of/h until the atmosphere in the furnace is replaced by inert gas and micro-positive pressure is maintained, and closing all gas inlets and outlets.
The fixed carbon content of the graphite treated by the experiment is 99.9995%. (high-temperature oxidation method is adopted, namely, accurately weighed high-purity graphite powder is filled into a platinum crucible, the platinum crucible is roasted at high temperature in an aerobic furnace at the temperature of 850-900 ℃, and fixed carbon in the graphite is oxidized at high temperature to generate CO2And weighing the residual substances, wherein the ratio of the weight loss to the weight of the original graphite powder is the fixed carbon content of the graphite powder, and a weighing instrument adopts a one ten-thousandth electronic balance).
Claims (10)
1. A graphite purification method, characterized in that the graphite purification method is as follows:
firstly, laying medium-carbon graphite or high-carbon graphite in a graphite crucible, then moving the graphite crucible into a high-temperature purification furnace, sealing the furnace body, and starting a vacuum pumping system until the absolute vacuum degree reaches 10 pa-100 pa;
secondly, heating to 800-1000 ℃, then preserving heat for 0.5-1 h, and introducing carbon tetrachloride at the flow rate of 0.5-1.5L/h while preserving heat;
thirdly, heating to 1200-1450 ℃, then preserving heat for 1-1.5 h, alternately introducing carbon tetrachloride and argon with the purity of 99.999% into the furnace while preserving heat, wherein the flow rate of introducing the carbon tetrachloride is 0.5L-1.5L/h, and the flow rate of introducing the high-purity argon is 2-3 m3/h；
The mode of alternately introducing carbon tetrachloride and argon with the purity of 99.999 percent into the furnace is as follows: after carbon tetrachloride is introduced for 10-15 min, closing an air inlet of the carbon tetrachloride, opening an argon inlet after 20-30 min, simultaneously opening an exhaust port, closing the exhaust port and the argon inlet after 30min, and repeatedly introducing carbon tetrachloride;
fourthly, heating to 1600-1800 ℃, then preserving heat for 1.5-2 h, alternately introducing carbon tetrachloride and argon with the purity of 99.999 percent into the furnace while preserving heat, wherein the flow rate of introducing the carbon tetrachloride is 0.5L-1.5L/h, and the flow rate of introducing the high-purity argon is 2-3 m3H, obtaining high-purity graphite;
the mode of alternately introducing carbon tetrachloride and argon with the purity of 99.999 percent into the furnace is as follows: and (3) after carbon tetrachloride is introduced for 10-15 min, closing an air inlet of the carbon tetrachloride, opening an argon inlet after 20-30 min, simultaneously opening an exhaust port, closing the exhaust port and the argon inlet after 30min, and repeatedly introducing carbon tetrachloride.
2. The method for purifying graphite according to claim 1, wherein the temperature rise rate in the first, second and third steps is 15 ℃/min.
3. The method for purifying graphite according to claim 1, wherein the temperature in the second step is raised to 800 ℃, and then the temperature is maintained for 0.5h, and carbon tetrachloride is introduced at a flow rate of 0.5L/h while the temperature is maintained.
4. The method for purifying graphite according to claim 1, wherein the temperature is raised to 900 ℃ in the second step, and then the temperature is maintained for 0.5h, and carbon tetrachloride is introduced at a flow rate of 1L/h while maintaining the temperature.
5. The method for purifying graphite according to claim 1, wherein the temperature is raised to 1000 ℃ in the second step, and then the temperature is maintained for 0.5h, and carbon tetrachloride is introduced at a flow rate of 1.5L/h while maintaining the temperature.
6. The method for purifying graphite as claimed in claim 1, wherein the temperature is raised to 1200 ℃ in the third step, and then the temperature is maintained for 1 hour, and carbon tetrachloride and argon gas with a purity of 99.999% are alternately introduced into the furnace while maintaining the temperature, the flow rate of carbon tetrachloride being 0.5L/h, and the flow rate of high purity argon gas being 2m3/h。
7. The method for purifying graphite as claimed in claim 1, wherein the temperature is raised to 1300 ℃ in the third step, and then the temperature is maintained for 1.5 hours, and carbon tetrachloride and argon gas with a purity of 99.999% are alternately introduced into the furnace while the temperature is maintained, wherein the flow rate of carbon tetrachloride is 1L/h, and the flow rate of high-purity argon gas is 2.5m3/h。
8. The method for purifying graphite as claimed in claim 1, wherein the temperature is raised to 1400 ℃ in the third step, and then the temperature is maintained for 1.5 hours, and carbon tetrachloride and argon gas with a purity of 99.999% are alternately introduced into the furnace while the temperature is maintained, wherein the flow rate of carbon tetrachloride is 1.5L/h, and the flow rate of high-purity argon gas is 3m3/h。
9. The method for purifying graphite as claimed in claim 1, wherein the temperature is raised to 1600 ℃ in the fourth step, and then the temperature is maintained for 1.5 hours, and carbon tetrachloride and argon gas with a purity of 99.999% are alternately introduced into the furnace while maintaining the temperature, the flow rate of carbon tetrachloride being 0.5L/h, and the flow rate of high purity argon gas being 2m3/h。
10. According to the claimsSolving 1 the graphite purification method is characterized in that the temperature is raised to 1700 ℃ in the fourth step, then the heat is preserved for 1.5h, carbon tetrachloride and argon with the purity of 99.999 percent are alternately introduced into the furnace while the heat is preserved, the flow rate of introducing the carbon tetrachloride is 0.8L/h, and the flow rate of introducing the high-purity argon is 2.3m3/h。
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