CN111228834B - High-vacuum continuous graphite purification device and application thereof - Google Patents
High-vacuum continuous graphite purification device and application thereof Download PDFInfo
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- CN111228834B CN111228834B CN202010097285.0A CN202010097285A CN111228834B CN 111228834 B CN111228834 B CN 111228834B CN 202010097285 A CN202010097285 A CN 202010097285A CN 111228834 B CN111228834 B CN 111228834B
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Abstract
The invention discloses a device for continuously purifying graphite in high vacuum and application thereof, belonging to the technical field of graphite purification. The method comprises the following steps: the device comprises a feeding chamber, a discharging chamber, a transmission device, an induction heating device, a level difference vacuum chamber and a pump set; the conveying device is horizontally arranged and conveys the raw materials to the discharging chamber from the feeding chamber during working; the induction heating device is arranged around the periphery of the transmission device; the heating section of the induction heating device is externally connected with an air pump set through a pipeline; the two sides of the heating section are provided with a stage difference vacuum chamber communicated with the heating section; the level difference vacuum chamber comprises 4-6 chambers, and the other ends of the chambers are communicated with a pump set through pipelines. According to the invention, only the graphite carbon passing through the heating part is heated, and meanwhile, the vacuum pumping is carried out in the purification process, so that the graphite purification temperature is reduced, and the purification efficiency is improved. In addition, the invention selects heating purification during the graphite conveying process, can continuously operate, and solves the problems that the continuous purification cannot be realized and the purification is insufficient and uniform in the prior art.
Description
Technical Field
The invention relates to the technical field of graphite purification, in particular to a high-vacuum continuous graphite purification device and application thereof.
Background
In the prior art, the method for purifying graphite mainly comprises the following steps: flotation, alkaline-acid, hydrofluoric acid, chlorination-roasting, and high temperature. Wherein, high temperature purification, i.e. physical purification, the graphite ore often contains Si2O3、Al2O3、MgO、Fe3O4And impurities such as CaO, and the like, wherein the impurities have high boiling points, and the boiling point temperature of MgO reaches 3600 ℃, so that inert protective gas needs to be introduced in the high-temperature heating and purifying process of graphite, and the product with the carbon content of more than 99.99 percent can be obtained only by increasing the heating temperature to more than 3000 ℃, thereby resulting in complex purification process and higher requirement on equipment.
In order to reduce the purification temperature, Cl is usually introduced into a high-temperature furnace in the prior art2And HCl and the like, so that impurities in the graphite are expected to react to generate low-boiling-point chloride, and the aim of separating the graphite from the impurities is fulfilled. Although the method can reduce the purification temperature, Cl2And HCl and the like are toxic, carbon powder is required to be added as a reducing agent in the reaction process, the operation is complex, and the production cost is high.
In addition, the traditional production method and production device have the problems of discontinuous production, low efficiency, more labor, and relatively high cost because each link in the middle needs to be operated by people. In addition, by adopting an intermittent production method, the temperature is too high when the materials are discharged, and the plastic layer on the inner lining of the fermented soya bean is easily heated and deformed after entering the centrifuge, so that the fermented soya bean is damaged, the maintenance is inconvenient, and the maintenance cost is increased.
Therefore, it is an urgent need to solve the problem of providing an apparatus capable of reducing the purification temperature of graphite and continuously purifying graphite.
Disclosure of Invention
In view of the above, the present invention provides a device capable of reducing the graphite purification temperature and continuously purifying graphite, and also provides an application of the device in graphite purification.
In order to achieve the purpose, the invention adopts the following technical scheme:
a high vacuum continuous purification graphite device, comprising: the feed chamber, ejection of compact room, its characterized in that still includes: the device comprises a transmission device, an induction heating device, a stage difference vacuum chamber and a pumping pump set;
the conveying device is horizontally arranged, and conveys the raw materials to the discharging chamber from the feeding chamber during working; the induction heating device is arranged around the periphery of the transmission device;
the heating section of the induction heating device is externally connected with the air pump set through a pipeline; a level difference vacuum chamber communicated with the heating section is arranged at two sides of the heating section; the level difference vacuum chamber comprises 4-6 chambers, and the other ends of the chambers are communicated with the air pump set through pipelines.
Preferably, the material of the conveying device is graphite.
The conveying belt is made of graphite, so that the conveying belt is high in resistance to high-temperature conditions in work, and even if the material of the conveying device is mixed into graphite due to scratch in the conveying process of graphite ore, the graphite product cannot be polluted by impurities.
Preferably, the vacuum degree in the chamber decreases from the center to two sides, and the vacuum degree in the chamber sequentially comprises one or more of an ultra-vacuum chamber, a high vacuum chamber and a low vacuum chamber.
An application of a high-vacuum continuous graphite purifying device in graphite purification.
Preferably, the graphite purification method comprises the steps of:
(1) preheating and vacuumizing: starting the induction heating device for preheating, and simultaneously starting a pumping pump set of the low vacuum chamber, wherein the pumping pump set is used for vacuumizing the low vacuum chamber through a pipeline;
(2) feeding: starting the conveying device to enable the conveying device to move at a constant speed, and feeding the graphite raw material into one end of the conveying device through the feeding chamber for conveying;
(3) and (3) purification: starting the air pump sets of the high vacuum chamber and the ultrahigh vacuum chamber, heating the graphite raw material in the step (2) by the induction heating device in the transmission process, and controlling the residence time of the graphite raw material at the induction heating device by controlling the transmission speed of the transmission device;
(4) discharging: and (4) conveying the graphite raw material purified in the step (3) to the discharge chamber by the conveying device for discharging to obtain a graphite product.
Preferably, the vacuum degree of the low vacuum chamber in the step (1) is 10-2-10Pa。
Preferably, the vacuum degree of the high vacuum chamber in the step (3) is 10-2-10-3Pa, the vacuum degree of the ultrahigh vacuum chamber is 10-3-10-4Pa。
Preferably, the preheating temperature in step (1) is 250-600 ℃.
Preferably, the heating temperature in step (3) is 1000-2000 ℃.
According to the invention, by arranging the vacuum chamber and limiting the vacuum degree of the vacuum chamber, the boiling point of impurities can be reduced, and the concentration of impurity steam in the vacuum chamber is reduced, so that the evaporation of the impurities is accelerated, and the purification temperature and the purification efficiency of graphite are improved.
According to the technical scheme, compared with the prior art, the induction heating device is arranged, only the graphite carbon passing through the heating part is heated, the heating efficiency of the equipment is improved, and the energy consumption is reduced. Meanwhile, the invention utilizes the multi-stage vacuum pump to ensure that the reaction device reaches a high vacuum state, so that the boiling point of impurities is reduced, and the purification temperature of graphite is further reduced. Finally, the invention can obtain high-purity graphite at the temperature below 2000 ℃. In addition, the graphite conveying device provided by the invention selects heating and purifying at the same time in the graphite conveying process, adjusts the heating time by controlling the conveying speed, achieves the purpose of improving the impurity removal rate without indirect feeding, and solves the problem that continuous purification cannot be realized in the prior art. Meanwhile, by using the device provided by the invention, the graphite purification process is simple, no reactive gas is required to be introduced, and the device is beneficial to industrial popularization.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a schematic view of an apparatus for continuous purification of graphite under high vacuum in example 1 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a device capable of reducing the graphite purification temperature and continuously purifying graphite, and also provides application of the device in graphite purification. The specific technical scheme is as follows:
a high vacuum continuous purification graphite device, comprising: a feeding chamber, a discharging chamber, an induction heating device, a transmission device, a level difference vacuum chamber and a pump set.
The conveying device is horizontally arranged and conveys the graphite ores to the discharging chamber from the feeding chamber during working; the induction heating device is arranged around the periphery of the transmission device; the heating section of the induction heating device is externally connected with an air pump set through a pipeline; the two sides of the heating section are provided with a stage difference vacuum chamber communicated with the heating section; the level difference vacuum chamber comprises 4-6 chambers which are communicated with a pump set through a pipeline.
The transmission device is made of graphite.
Preferably, the vacuum degree in the chamber decreases from the center to two sides, and the vacuum degree in the chamber sequentially comprises one or more of an ultra-vacuum chamber, a high vacuum chamber and a low vacuum chamber.
An application of a high-vacuum continuous graphite purifying device in graphite purification.
Preferably, the graphite purification method comprises the steps of:
(1) preheating and vacuumizing: starting the induction heating device for preheating, and simultaneously starting a pumping pump set of the low vacuum chamber, wherein the pumping pump set is used for vacuumizing the low vacuum chamber through a pipeline;
(2) feeding: starting the conveying device to enable the conveying device to move at a constant speed, and feeding the graphite raw material into one end of the conveying device through the feeding chamber for conveying;
(3) and (3) purification: starting the air pump sets of the high vacuum chamber and the ultrahigh vacuum chamber, heating the graphite raw material in the step (2) by the induction heating device in the transmission process, and controlling the residence time of the graphite raw material at the induction heating device by controlling the transmission speed of the transmission device;
(4) discharging: and (4) conveying the graphite raw material purified in the step (3) to the discharge chamber by the conveying device for discharging to obtain a graphite product.
Preferably, the vacuum degree of the low vacuum chamber in the step (1) is 10-2-10Pa。
Preferably, the vacuum degree of the high vacuum chamber in the step (3) is 10-2-10-3Pa, the vacuum degree of the ultrahigh vacuum chamber is 10-3-10-4Pa。
Preferably, the preheating temperature in step (1) is 250-600 ℃.
Preferably, the heating temperature in step (3) is 1000-2000 ℃.
Example 1:
a high vacuum continuous graphite purifying apparatus, as shown in fig. 1, comprising: the device comprises a feeding chamber 1, a discharging chamber 2, an induction heating device 3, a transmission device 4, a stage difference vacuum chamber 5 and a pump set 6.
The conveying device 4 is horizontally arranged and is made of graphite. During working, the graphite ore is transported from the feeding chamber 1 to the discharging chamber 2; the induction heating device 3 is arranged around the periphery of the transmission device 4; the heating section of the induction heating device 3 is externally connected with an air pump set 6 through a pipeline; the two sides of the heating section are provided with a level difference vacuum chamber 5 communicated with the heating section; the stage difference vacuum chamber 5 comprises 5 chambers, the vacuum degree in the chambers decreases from the center to two sides, and the chambers sequentially comprise an ultra-vacuum chamber 51, a high vacuum chamber 52 and a low vacuum chamber 53. The chamber is communicated with the group of the air suction pumps 6 through a pipeline.
An application of an ultrahigh vacuum continuous graphite purifying device in graphite purification comprises the following steps:
(1) preheating and vacuumizing: starting an induction heating device 3 for preheating, wherein the preheating temperature is 500 ℃; simultaneously, the air pump set of the low vacuum chamber 53 is started, and the air pump set vacuumizes the chamber of the stage difference vacuum chamber 5 through a pipeline, wherein the vacuum degree is 10-2Pa；
(2) Feeding: starting the conveying device 4 to enable the conveying device 4 to move at a constant speed, and feeding the graphite raw material into one end of the conveying device 4 through the feeding chamber 1 for conveying;
(3) and (3) purification: opening the air-pump set of the high vacuum chamber and the ultra-high vacuum chamber to make the vacuum degree in the high vacuum chamber 10-2Pa, degree of vacuum in the ultra-high vacuum chamber of 10-4Pa. Heating the graphite raw material in the step (2) by an induction heating device 3 in the transmission process, wherein the heating temperature is 2000 ℃, and controlling the retention time of the raw material at the induction heating device 3 by controlling the transmission speed of a transmission device 4;
(4) discharging: and (4) after the purification of the graphite raw material in the step (3) is finished, conveying the product to the discharge chamber 2 by the conveying device 4 to discharge, and thus obtaining the graphite product.
Example 2:
a high vacuum continuous graphite purifying device, which is different from the embodiment 1:
the level difference vacuum chamber 5 comprises 4 chambers which are communicated in sequence.
The application of the high-vacuum continuous graphite purifying device in graphite purification is different from the application of example 1 in that:
1) the induction heating device in the step (1) is heated by a silicon-molybdenum rod, and the preheating temperature is 450 ℃;
2) the step (3) does not include an ultrahigh vacuum chamber, and the vacuum degree in the ultrahigh vacuum chamber is 10-3Pa；
3) The heating temperature in step (3) was 1800 ℃.
Example 3:
a high vacuum continuous graphite purification apparatus, the same as the apparatus described in example 1.
The application of the high-vacuum continuous graphite purifying device in graphite purification is different from the application of example 1 in that:
1) the heating mode of the induction heating device in the step (1) is heating by an induction heating coil, and the preset heating temperature is 600 ℃;
2) the vacuum degree of the low vacuum chamber in the step (1) is 10 Pa;
3) the vacuum degree of the ultrahigh vacuum chamber in the step (3) is 10-3Pa；
4) The heating temperature in the step (3) was 1200 ℃.
Example 4:
an ultrahigh vacuum continuous graphite purifying device is different from the embodiment 1 in that:
the level difference vacuum chamber 5 comprises 6 chambers which are communicated in sequence.
The application of the high-vacuum continuous graphite purifying device in graphite purification is different from the application of example 1 in that:
1) the heating mode of the induction heating device in the step (1) is heating by an induction heating coil, and the preset heating temperature is 580 ℃;
2) the vacuum degree of the low vacuum chamber in the step (1) is 1 Pa;
3) the vacuum degree of the ultrahigh vacuum chamber in the step (3) is 10-3Pa, highVacuum chamber vacuum degree of 10-3Pa；
4) The heating temperature in step (3) was 1500 ℃.
Example 5:
a high vacuum continuous graphite purifying device, which is different from the embodiment 1:
the level difference vacuum chamber 5 comprises 6 chambers which are communicated in sequence.
The application of the high-vacuum continuous graphite purifying device in graphite purification is different from the application of example 1 in that:
1) the heating mode of the induction heating device in the step (1) is heating by an induction heating coil, and the preset heating temperature is 470 ℃;
2) the vacuum degree of the low vacuum chamber in the step (1) is 1 Pa;
3) the vacuum degree of the ultrahigh vacuum chamber in the step (3) is 10-4Pa, vacuum degree of the high vacuum chamber is 10-3Pa；
4) The heating temperature in the step (3) was 1600 ℃.
Example 6:
a high vacuum continuous graphite purifying device, which is different from the embodiment 1:
the level difference vacuum chamber 5 comprises 4 chambers which are communicated in sequence.
The application of the high-vacuum continuous graphite purifying device in graphite purification is different from the application of example 1 in that:
1) the preset vacuum degree of the stage difference vacuum chamber 5 in the step (1) is 10-2Pa；
2) The heating mode of the induction heating device in the step (1) is heating by an induction heating coil, and the preset heating temperature is 530 ℃;
3) the step (3) does not include an ultrahigh vacuum chamber, and the vacuum degree of the ultrahigh vacuum chamber is 10-2Pa；
4) The heating temperature in step (3) was 1300 ℃.
Example 7:
a high vacuum continuous graphite purifying device, which is the same as the device in the embodiment 1.
The application of the high-vacuum continuous graphite purifying device in graphite purification is different from the application of example 1 in that:
1) the heating mode of the induction heating device in the step (1) is heating by an induction heating coil, and the preset heating temperature is 550 ℃;
2) the vacuum degree of the low vacuum chamber in the step (1) is 0.1 Pa;
3) the vacuum degree of the ultrahigh vacuum chamber in the step (3) is 10-3Pa, vacuum degree of the high vacuum chamber is 10-2Pa；
4) The heating temperature in step (3) was 1100 ℃.
Example 8:
a high vacuum continuous graphite purifying device, which is different from the embodiment 1:
the level difference vacuum chamber 5 comprises 6 chambers which are communicated in sequence.
The application of the high-vacuum continuous graphite purifying device in graphite purification is different from the application of example 1 in that:
1) the heating mode of the induction heating device in the step (1) is heating by an induction heating coil, and the preset heating temperature is 570 ℃;
2) the vacuum degree of the low vacuum chamber in the step (1) is 10 Pa;
3) the vacuum degree of the ultrahigh vacuum chamber in the step (3) is 10-3Pa；
4) The heating temperature in step (3) was 1700 ℃.
Comparative example 1
A high vacuum continuous graphite purifying device, which is different from the embodiment 1:
the heating mode does not adopt an induction heating device to directly heat the raw materials on the conveying device, but uses a heating furnace, and the heating temperature is higher than 3000 ℃.
According to the method, the graphite ore is required to stay in the heating furnace, so that the continuous purification of the graphite cannot be achieved, the purification time of the graphite is prolonged, and the energy consumption is increased.
Comparative example 2
A high vacuum continuous graphite purifying device, which is different from the embodiment 1:
the device does not comprise a step vacuum chamber and a pump set, namely, the vacuumizing operation is not adopted.
Technical effects
The carbon contents of the graphite products obtained by the above examples and comparative examples are shown in table 1:
table 1:
| carbon content (%) | |
| Example 1 | 99.9999 |
| Example 2 | 99.99 |
| Example 3 | 99.92 |
| Example 4 | 99.95 |
| Example 5 | 99.98 |
| Example 6 | 99.98 |
| Example 7 | 99.9 |
| Example 8 | 99.999 |
| Comparative example1 | 99.99 |
| Comparative example 2 | 89 |
As can be seen from the data in Table 1, the carbon content of the graphite product obtained by the method in the comparative example is far lower than that of the present invention, while the heating temperature of the comparative example needs to be adjusted to 3000 ℃ or higher if the graphite product with the carbon content of 99.9% or more is obtained. Therefore, the method provided by the invention can greatly improve the purity of the graphite product, and can obviously reduce energy consumption in the production process, thereby greatly reducing the production cost, and being suitable for industrial popularization.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. The device disclosed by the embodiment corresponds to the method disclosed by the embodiment, so that the description is simple, and the relevant points can be referred to the method part for description.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (4)
1. A high vacuum continuous purification graphite device, comprising: the feed chamber, ejection of compact room, its characterized in that still includes: the device comprises a transmission device, an induction heating device, a stage difference vacuum chamber and a pumping pump set;
the conveying device is horizontally arranged, and conveys the raw materials to the discharging chamber from the feeding chamber during working; the induction heating device is arranged around the periphery of the transmission device;
the heating section of the induction heating device is externally connected with the air pump set through a pipeline; a level difference vacuum chamber communicated with the heating section is arranged at two sides of the heating section; the level difference vacuum chamber comprises 4-6 chambers, and the other ends of the chambers are communicated with the air pump set through pipelines;
the transmission device is made of graphite;
the vacuum degree in the chamber is gradually decreased from the center to two sides, and the chamber sequentially comprises an ultrahigh vacuum chamber, a high vacuum chamber and a low vacuum chamber;
the application of the high-vacuum continuous graphite purifying device in graphite purification comprises the following steps:
(1) preheating and vacuumizing: starting the induction heating device for preheating, and simultaneously starting a pumping pump set of the low vacuum chamber, wherein the pumping pump set is used for vacuumizing the low vacuum chamber through a pipeline;
(2) feeding: starting the conveying device to enable the conveying device to move at a constant speed, and feeding the graphite raw material into one end of the conveying device through the feeding chamber for conveying;
(3) and (3) purification: starting the air pump sets of the high vacuum chamber and the ultrahigh vacuum chamber, heating the graphite raw material in the step (2) by the induction heating device in the transmission process, and controlling the residence time of the graphite raw material at the induction heating device by controlling the transmission speed of the transmission device;
(4) discharging: conveying the graphite raw material purified in the step (3) to the discharging chamber by the conveying device for discharging to obtain a graphite product;
the heating temperature in the step (3) is 1000-.
2. The apparatus for continuous purification of graphite under high vacuum as claimed in claim 1, wherein the preheating temperature in step (1) is 250-600 ℃.
3. The method of claim 1The high-vacuum continuous graphite purification device is characterized in that the vacuum degree of the low-vacuum chamber in the step (1) is 10-2-10Pa。
4. The apparatus for continuous purification of graphite in high vacuum according to claim 3, wherein the degree of vacuum of the high vacuum chamber in step (3) is 10-2-10-3Pa, the vacuum degree of the ultrahigh vacuum chamber is 10-3-10-4Pa。
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| GB455185A (en) * | 1935-01-05 | 1936-10-15 | British Thomson Houston Co Ltd | Improvements in and relating to methods of purifying graphite |
| CN2690373Y (en) * | 2004-04-26 | 2005-04-06 | 朱兴发 | Vacuum high temperatare continuous micro crystal graphite purifting producing device |
| CN103172060B (en) * | 2013-04-15 | 2013-11-13 | 文中华 | Continuous industrialized natural graphite purification equipment |
| CN106064815B (en) * | 2016-06-01 | 2017-11-07 | 陕西六元碳晶股份有限公司 | The high-purity graphite powder that the method and this method of graphite powder purification are prepared |
| CN207294185U (en) * | 2017-07-06 | 2018-05-01 | 咸阳非金属矿研究设计院有限公司 | One new type of continuous high temperature method graphite purification equipment |
| CN207079010U (en) * | 2017-07-21 | 2018-03-09 | 黑龙江省牡丹江农垦奥宇石墨深加工有限公司 | A kind of novel graphite continuously purification device |
| CN109292768A (en) * | 2018-11-23 | 2019-02-01 | 湖南顶立科技有限公司 | A kind of high purity graphite powder and its purifying technique |
| CN109941993A (en) * | 2019-04-15 | 2019-06-28 | 北京航空航天大学 | A kind of method of high vacuum low temperature purification graphite |
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