CN217297311U

CN217297311U - Novel graphite powder multistage control degree of depth purification device

Info

Publication number: CN217297311U
Application number: CN202220032696.6U
Authority: CN
Inventors: 王宁; 刘骏; 雷光雄; 高定; 李玥鹏
Original assignee: Beijing Lvqing Technology Co ltd
Current assignee: Beijing Lvqing Technology Co ltd
Priority date: 2022-01-07
Filing date: 2022-01-07
Publication date: 2022-08-26
Anticipated expiration: 2032-01-07

Abstract

The utility model discloses a novel graphite powder multistage sub-control depth purification device, which comprises a purification unit, a cooling unit and a tail gas treatment unit, wherein high-temperature high-purity graphite produced by the purification unit is further cooled in the cooling unit to obtain a high-purity graphite powder product; tail gas generated by the purification unit enters a tail gas treatment unit, is purified and separated into purified gas and inert gas, and is recycled to the purification unit to continuously participate in the purification production of graphite powder; high-temperature and high-pressure steam generated by heat exchange of the cooling unit is supplied to the steam power generation system for power generation, and power generated by the steam power generation system is supplied to the purification unit for heating. The multi-stage separate control deep purification device for the graphite powder realizes the continuous purification production of the high-purity graphite powder, and improves the product purity, the production rate and the production scale; the tail gas generated by the purification unit is subjected to heat recovery to supply power for the purification process, and the tail gas is recovered and separated to be used for the purification process of the graphite powder raw material, so that the energy consumption is saved, and the pollution is reduced.

Description

Novel graphite powder multistage control degree of depth purification device

Technical Field

The utility model relates to a novel graphite powder is multistage to be divided accuse degree of depth purification device for produce the high-purity graphite more than 99.999% of purity, belong to graphite powder purification device field.

Background

In recent years, with the continuous development of high and new technology in the graphite industry, the general high-purity graphite product cannot meet the requirements of various industries, and the graphite needs to be purified to more than 99.999% to produce the high-purity graphite. The high-purity graphite is not only a basic raw material of modern high-temperature, high-pressure and high-speed industries and modern biology, information and energy, but also a key material and a multifunctional environment-friendly material of modern high and new technology industries, and is an indispensable strategic material in the fields of nuclear energy, aerospace, national defense and military.

The main impurity components contained in the graphite powder raw material for industrially producing the high-purity graphite are silicate minerals such as K, Na, Mg, Fe, Ca and the like, which can be effectively removed by a high-temperature method, but only the high-purity graphite with the purity of 99.99-99.999 percent can be produced by the high-temperature method. This is because although the high temperature method can remove impurities such as Fe, Ca, Na, etc. and compounds thereof, B, Al, V are also liable to form high melting point and high boiling point carbides such as B4C, VC, etc., which are not removed under high temperature conditions. At present, a fixed bed (namely a graphite crucible) intermittent staged temperature control purification mode is commonly adopted in a device for producing high-purity graphite in batches, so that the operation time for producing graphite powder is increased, and the produced high-purity graphite product has purity difference in the radial direction and the axial direction of the fixed bed; the existing device for continuously producing the high-purity graphite also has the defects of unstable product purity, unorganized tail gas emission and the like.

The device for purifying graphite at high temperature by a physical method at home and abroad comprises a graphite crucible, an Acheson furnace, a flotation column, graphite alkali melting equipment and the like. The advantages and disadvantages of various production facilities are as follows:

(1) high-temperature graphite crucible:

the high-temperature graphite crucible belongs to equipment for producing high-purity graphite by intermittent staged temperature control, and is a main mode for producing high-purity graphite powder in small batches at present. However, the device for producing high-purity graphite not only increases the operation time for producing graphite powder, but also produces high-purity graphite products with purity difference in the radial direction and the axial direction of the fixed bed. In the process of producing high-purity graphite by using the high-temperature graphite crucible, the graphite powder raw material is heated in an inert atmosphere and does not flow, the production period is 6-7 days, and the energy consumption is high; and generally adopts a fixed bed intermittent operation mode, and has the problems of poor reaction and heat transfer effects and uneven purification purity of graphite products easily formed in the longitudinal direction and the radial direction of a graphite crucible; the batch method and the small-batch production scale are adopted, and the continuous production of the high-purity graphite and the temperature control of each stage are not realized.

(2) Acheson furnace:

the Acheson furnace belongs to equipment for producing graphite powder by high-temperature physical purification, and has the advantages of simple equipment and large yield, but has certain disadvantages: long production period, different quality in different areas, unorganized exhaust emission and serious pollution. Because the Acheson furnace has serious environmental pollution and great harm to human bodies, the application of the Acheson furnace is strictly limited at present; and has the disadvantages of long equipment period, high energy consumption, low yield and difficult large-scale production.

(3) A flotation column:

the graphite powder raw material is purified by a flotation method. The flotation column is a cylindrical flotation device, has the characteristics of energy conservation, small floor area, high grade of ore dressing concentrate, large ore dressing ratio and the like, is a key device for realizing short-flow flotation of graphite and improving the grade of graphite ore dressing concentrate, and the purity of the produced graphite product is less than 99.999 percent.

(4) Graphite alkali melting equipment:

the alkaline-acid method is a method widely applied in the industrial production of graphite purification in China, and has the characteristics of low one-time investment, high product grade, strong adaptability and the like. The traditional graphite alkali melting equipment has small output and small production scale.

In conclusion, the existing graphite purifying devices have different disadvantages, and need to be improved.

SUMMERY OF THE UTILITY MODEL

The utility model aims at providing a novel graphite powder is multistage to divide accuse degree of depth purification device to solve the problem that the mass transfer heat transfer that prior art exists is inhomogeneous, purification purity is low, the production scale is little and waste heat recovery utilization ratio is low, also realize serialization, the large-scale production process and each purification stage temperature of high-purity graphite powder simultaneously and control.

In order to achieve the above object, the present invention adopts the following main technical solutions:

a novel graphite powder multistage separate control deep purification device comprises a purification unit, a cooling unit and a tail gas treatment unit, wherein a high-purity graphite powder outlet of the purification unit is connected with a high-purity graphite powder inlet of the cooling unit through a blocking material returning device, and a purified gas outlet of the purification unit is connected with an input end of the tail gas treatment unit; the high-temperature and high-purity graphite produced by the purification unit is further cooled in a cooling unit to obtain a high-purity graphite powder product; tail gas generated by the purification unit enters a tail gas treatment unit, is purified and separated into purified gas and inert gas, and is recycled to the purification unit to continuously participate in the purification production of graphite powder; high-temperature and high-pressure steam generated by heat exchange of the cooling unit is supplied to the steam power generation system for power generation, and power generated by the steam power generation system is supplied to the purification unit for heating.

As a preferred embodiment of the utility model, the purifying unit comprises a cyclone purifier, a circulating purifier and a deep purifier; the system comprises a cyclone purifier, a graphite powder raw material bin, a purified gas bin, a circulating purifier, a purified gas inlet, a gas outlet, a gas inlet, a gas outlet, a gas inlet and a gas outlet, wherein the graphite powder raw material and the purified gas inlet are connected with the outlet of the graphite powder raw material bin; the secondary purified graphite powder and the purified gas outlet at the upper part of the circulating purifier are sequentially connected with a secondary purified graphite return port at the lower part of the circulating purifier through a separator and a material returning device to form a circulating purification loop; the bottom end of the separator is connected with a secondary purified graphite powder inlet in the middle of the deep purifier through a dipleg, a high-purity graphite powder outlet at the bottom end of the deep purifier is connected with a high-purity graphite powder inlet of the blocking returning feeder, a purified gas air hole of the deep purifier is connected with a gas outlet at the top end of the separator, and a purified gas outlet of the deep purifier is connected with the tail gas treatment unit.

As a preferred embodiment of the present invention, the cyclone purifier includes a cyclone purifier housing having a closed cylindrical top end, a coaxial purified gas exhaust pipe is disposed at the middle upper portion inside the cyclone purifier housing, a bell mouth is disposed at the top end of the purified gas exhaust pipe, and an exhaust pipe outlet obliquely led out from the side surface of the cyclone purifier housing is disposed at the lower end of the purified gas exhaust pipe; the bottom of the shell of the cyclone purifier is provided with a first purified graphite powder outlet and a discharge stirring screw.

As a preferred embodiment of the present invention, the circulation purifier includes a closed cylindrical circulation purifier housing, a gas distribution pipe, a purified gas bottom inlet and a secondary purified graphite return port are respectively disposed in the bottom and at the bottom of the circulation purifier housing, and a primary purified graphite powder inlet and a purified gas side interface are respectively disposed from bottom to top on the circulation purifier housing above the gas distribution pipe; the top of the shell of the circular purifier is provided with a secondary purified graphite powder outlet and a purified gas outlet.

As a preferred embodiment of the present invention, the purified gas side interface is disposed on 1-3 circulation pipes, a plurality of circulation pipes surround the periphery of the shell of the circulation purifier, and the axial distance between more than two circulation pipes is 0.5-1.5 m; and a plurality of air inlet pipes which obliquely penetrate into the shell of the circular purifier downwards are uniformly connected to the circular flow pipe along the circumference, and the included angle alpha between each air inlet pipe and the horizontal direction is 10-15 degrees.

As a preferred embodiment of the present invention, the deep purifier comprises a V-shaped fluidization section, a baffling purification section and a suspension purification section which are sequentially connected from bottom to top, wherein a conical air distribution plate is arranged in the V-shaped fluidization section, and an included angle β between the V-shaped fluidization section and a horizontal plane is 45-60 °; air holes are arranged on the conical air distribution plate at intervals, the diameter of each air hole is 2-6 mm, and the distance between the air holes is 0.5-1.0 time of the diameter of each air hole; the bottom end of the conical air distribution plate is butted with a high-purity graphite powder outlet arranged at the bottom end of the deep purifier; a plurality of purified gas air holes are formed in the side surface of the bottom of the deep purifier along the periphery; a plurality of guide cylinders with the same inclination angle as the conical air distribution plate are arranged in the baffling purification section, and the guide cylinders are arranged in the baffling purification section in a staggered mode; the baffling purification section is provided with a secondary purified graphite powder inlet which is connected with the dipleg; the diameter of the suspension purification section is larger than that of the baffling purification section, and the suspension purification section and the baffling purification section are in transitional connection through a cone; and a purified gas outlet is arranged at the top of the suspension purification section and is connected with the tail gas treatment unit.

As a preferred embodiment of the present invention, the cooling unit comprises a cooler and an air cooling system, wherein the outlet of the cooler for cooling the high purity graphite powder is connected with the inlet of the air cooling system; a high-purity graphite powder inlet of the cooler is connected with a to-be-cooled high-purity graphite powder outlet of the blocking returning feeder; the inlet of a cooling medium channel of the cooler is connected with the cooling medium outlet of the heat exchanger through a pipeline; and the steam outlet of the cooler is connected with a steam power generation system.

As a preferred specific embodiment of the utility model, the tail gas treatment unit comprises a settling chamber, a heat exchanger, a water scrubber, an alkaline tower, a condensation chamber and a gas separator which are sequentially connected through pipelines; wherein the inlet of the settling chamber is connected with the purified gas outlet of the deep purifier; a deoxidized water inlet of the heat exchanger is used for being connected with a cooling medium, and a cooling medium outlet of the heat exchanger is connected with a cooling medium channel inlet of the cooler through a pipeline; a third outlet of the condensing chamber is a condensed water outlet; the gas separator is provided with two outlets, namely a purified gas outlet and an inert gas recycling outlet, and the purified gas outlet is connected with the graphite powder raw material and the purified gas inlet of the cyclone purifier; and a purified gas adding port is arranged at the purified gas outlet.

As a preferred embodiment of the present invention, the steam outlet of the cooler is connected to a steam power generation system, and the steam power generation system is provided with a low-temperature steam outlet.

The utility model discloses a main advantage includes:

(1) graphite powder raw materials in each purifier of the purification unit can be purified in the basically constant purified gas concentration, the reaction rate is improved, meanwhile, the continuous purification production of high-purity graphite powder is realized through the serial operation of a plurality of graphite powder purifiers, the production time is shortened to 2-4 h, and the production scale is improved.

(2) The tail gas generated by the purification unit is subjected to heat recovery to supply power for the graphite powder raw material purification process, and is recycled and separated for the graphite powder raw material purification process, so that the energy recovery and resource recycling of the graphite powder purification process are realized.

(3) Each purifier of the purification unit adopts the flowing contact reaction of gas and graphite powder, thereby improving the mixing heat transfer and reaction efficiency and ensuring the stable purity of the produced high-purity graphite powder product.

Drawings

Fig. 1 is a schematic overall configuration diagram of an embodiment of the present invention;

FIG. 2 is a schematic diagram of the cyclone purifier of FIG. 1;

FIG. 3 is a schematic diagram of the configuration of the recycle purifier of FIG. 1;

FIG. 4 is a schematic diagram of the deep purifier of FIG. 1;

FIG. 5 is a schematic view of the structure of the blocking return feeder in FIG. 1;

fig. 6 is a schematic view of the cooler of fig. 1.

Description of reference numerals: 1. graphite powder raw material bin, 2, cyclone purifier, 3, stock bin, 4, circulating purifier, 5, separator, 6, return feeder, 7, deep purifier, 8, settling chamber, 9, heat exchanger, 10, water washing tower, 11, alkali washing tower, 12, condensing chamber, 13, gas separator, 14, cooler, 15, steam power generation system, 16, air cooling system, 17, raw material bin inert gas inlet, 18, graphite powder raw material inlet, 19, purified gas exhaust pipe, 191, bell mouth, 192, exhaust pipe outlet, 20, cyclone purifier inert gas inlet, 21, return feeder inert gas inlet, 22, blocking return feeder inert gas inlet, 23, inert gas inlet at the bottom of cooler, 24, cooled inert gas outlet, 25, high-purity graphite powder outlet, 26, low-temperature steam outlet, 27, power output, 28, deoxygenated water inlet, 29. purified gas adding port, 30, purified gas outlet, 31, inert gas recycling outlet, 32, condensed water outlet, 33, graphite powder raw material and purified gas inlet, 34, discharge stirring screw, 35, exhaust port blocking head, 36, primary purified graphite powder outlet, 37, dipleg, 38, blocking returning device, 41, primary purified graphite powder inlet, 42, gas distribution pipe, 43, purified gas bottom inlet, 44, purified gas side interface, 45, secondary purified graphite powder and purified gas outlet, 46, circulating pipe, 47, secondary purified graphite returning port, 71, secondary purified graphite powder inlet, 72, purified gas air hole, 73, high-purity graphite powder outlet, 74, purified gas outlet, 75, conical air distribution plate, 76, guide cylinder, 141, cooling medium channel inlet, 142, steam outlet, 143 and cooler high-purity graphite powder inlet, 144. the device comprises a cooling high-purity graphite powder outlet of a cooler, 145, a cooler water-cooled wall, 381, a sealing return feeder high-purity graphite powder inlet, 382 and a to-be-cooled high-purity graphite powder outlet of a sealing return feeder.

Detailed Description

Referring to fig. 1-6, the utility model relates to a novel graphite powder multistage separation control depth purification device, which comprises a purification unit, a cooling unit and a tail gas treatment unit, wherein the high-temperature and high-purity graphite produced by the purification unit is further cooled in the cooling unit to obtain a high-purity graphite powder product; tail gas generated by the purification unit enters a tail gas treatment unit, is purified and separated into purified gas and inert gas, and is recycled to the purification unit to continuously participate in the purification production of graphite powder; high-temperature and high-pressure steam generated by heat exchange of the cooling unit is supplied to the steam power generation system for power generation, and power generated by the steam power generation system is supplied to the purification unit for heating.

The production of high-temperature and high-purity graphite is realized in the purification unit by the graphite powder raw material, and the produced high-temperature and high-purity graphite is further cooled in the cooling unit to obtain a high-purity graphite powder product; tail gas generated by the purification unit enters a tail gas treatment unit, is purified and separated into purified gas and inert gas, and is recycled to the purification unit to continuously participate in the purification production of graphite powder; the deoxygenated water enters a cooling unit for dividing wall type heat exchange to generate high-temperature high-pressure steam to be used for generating power for a purification unit to be used for electric heating.

The structure and the working process of the utility model are further explained by the following combination and the attached drawings: graphite powder raw materials are conveyed to a graphite powder raw material bin 1, and raw materials are added in real time according to a material level meter in the graphite powder raw material bin 1, so that the graphite powder raw materials in the graphite powder raw material bin 1 are always kept at a certain material level. The lower part of the graphite powder raw material bin 1 is provided with a raw material bin inert gas inlet 17 for inputting low-pressure inert gas (mainly argon), and the low-pressure inert gas is used for pneumatically conveying graphite powder raw materials to enter the purification device.

And the cyclone purifier 2, the circulating purifier 4 and the deep purifier 7 in the purification unit are controlled in temperature by adopting an electric heating mode. Graphite powder raw materials firstly enter a cyclone purifier 2 in a pneumatic conveying mode to be purified to produce primary purified graphite powder; the primary purified graphite powder in the bin 3 at the lower part of the cyclone purifier 2 is pneumatically conveyed into the circulating purifier 4 to further purify the primary purified graphite powder in the cyclone purifier 2 into secondary purified graphite powder, and the secondary purified graphite powder in the circulating purifier 4 is returned into the circulating purifier 4 through the separator 5 and the material returning device 6 in sequence, so that the circulating purification in the circulating purifier 4 is realized; qualified secondary purified graphite powder produced in the circulating purifier 4 is sent into the deep purifier 7 through a dipleg 37 at the lower part of the separator 5, and the secondary purified graphite powder output from the separator 5 is respectively distributed into the material returning device 6 and the deep purifier 7 through the pressure self-balancing of the purifying device; and the secondary purified graphite powder is purified for the third time in the deep purifier 7 to produce high-purity graphite powder with the purity higher than 99.999 percent.

The cyclone purifier 2 adopts a purification mode of downward discharge of purified gas and graphite powder raw material by forward flow reaction. Graphite powder raw materials enter the cyclone purifier 2 at an inclined horizontal angle of 15-30 degrees at a gas speed of 40-60 m/s under pneumatic carrying of purified gas (including inert gas and purified gas). Purified gas carrying graphite powder raw materials rotates downwards in the cyclone purifier 2, most of the purified gas rotates to the purified gas exhaust pipe 19 to be discharged, the other small part of the purified gas continues to rotate downwards, the flow direction is turned when the purified gas reaches the bottom plate, the purified gas moves upwards to the exhaust pipe outlet 192 of the purified gas exhaust pipe 19 against the exhaust pipe to be discharged, and the separated primary purified graphite powder enters the bin 3 at the lower part of the cyclone purifier 2. The lower part of the cyclone purifier 2 is provided with a discharge stirring screw 34 which is used for carrying out moving bed type purification treatment on the primary purified graphite powder purified by the cyclone purifier 2 and ensuring that the primary purified graphite powder is not easy to fill and block at the bottom of the cyclone purifier. The purification process of the cyclone purifier 2 for the graphite powder raw material belongs to the coupling purification of cyclone and movement. The upper part of a purified gas exhaust pipe 19 of the cyclone purifier 2 is provided with an upward bell-mouth 191 shape to promote the purified gas to form extraction, further separate the primary purified graphite powder in the purified gas and ensure that less primary purified graphite powder is carried in the purified gas.

The circulating purifier 4 is used for circularly purifying the primary purified graphite powder produced in the cyclone purifier 2 to produce secondary purified graphite powder. The purified gas separated by the cyclone purifier 2 enters the circulating purifier 4 in two paths, one path enters the bottom of the circulating purifier 4 through a purified gas bottom inlet 43, the other path enters a circulating pipe 46 on the side surface of the lower part of the circulating purifier 4 through a plurality of purified gas side interfaces 44, and the volume ratio of the inlet gas of the two paths is controlled to be 2: 1-3: 2. The purified gas entering the bottom of the circulation purifier 4 enters the circulation purifier 4 through the distribution pipe 42 arranged at the lower part of the circulation purifier 4, and the distribution pipe 42 is uniformly arranged at the bottom of the circulation purifier 4 in a bouquet shape. The gas velocity of the purified gas in the distribution pipe 42 is controlled to be 40-60 m/s, so that the graphite powder purified at one time can not be deposited at the bottom of the circulating purifier 4. Purified gas entering a furnace body at the lower part of the circular purifier 4 enters a plurality of layers of circulating pipes 46 surrounding the periphery of the lower part of the circular purifier 4, the number of the layers is generally 1-3, and the interval of each layer of circulating pipes 46 is 0.5-1.5 m along the height direction of the circular purifier 4. The circulating pipes 46 are uniformly provided with 3-6 air inlet pipes which enter the furnace body, the included angle alpha between each layer of circulating pipe and the horizontal direction is 10-15 degrees, and the air speed in each air inlet pipe is controlled at 30-40 m/s. The circulation tube 46 arranged in the circulation purifier 4 for purifying gas can ensure that the concentration of the gas participating in purification in the circulation purifier 4 for purifying the graphite powder for the first time is uniform, and can regulate and control the purification time of the graphite powder for the first time in the circulation purifier 4 in a single circulation manner.

The deep purifier 7 is divided into three sections which are sequentially connected from bottom to top: a V-shaped fluidization section (I), a baffling purification section (II) and a suspension purification section (III). The V-shaped fluidization section (I) is mainly used for introducing the purified gas separated by the circulating purifier 4 into the deep purifier 7 through a purified gas air hole 72 at the lower part of the deep purifier 7, and performing fluidization purification reaction with the secondary purified graphite powder entering the deep purifier 7 from the dipleg 37 at the lower part of the separator 5 through a secondary purified graphite powder inlet 71. The lower part of the deep purifier 7 is provided with a conical air distribution plate 75, and the included angle beta between the conical air distribution plate and the horizontal plane is 45-60 degrees. Uniformly distributed air holes are formed in the conical air distribution plate 75, 3-5 layers of circular air holes are formed in the conical air distribution plate, the diameter of each air hole is 2-6 mm, the distance between every two layers of air holes is 0.5-1.0 time of the diameter of each air hole, and the speed of purified gas in each air hole is controlled to be 30-45 m/s; the baffling purification section (II) is internally provided with guide cylinders 76 with the same inclination angle as the conical air distribution plate 75, and the guide cylinders 76 are in a staggered arrangement mode, so that the heat transfer and mass transfer disturbance degree of the secondary purified graphite powder and the purified gas is increased, and the purity uniformity of the purified product graphite powder 3 is improved. The diameter of the suspension purification section (III) is enlarged, the purpose is to reduce the carrying amount of the secondary purified graphite powder carried by the purified gas, the gas velocity of the purified gas is controlled to be 0.05-0.10 m/s, and the loss of the secondary purified graphite powder in the deep purifier is reduced. Discharging high-purity graphite powder (with the purity of more than 99.999%) produced in the deep purifier 7 according to the pressure difference delta P between the upper part and the lower part of the baffling purification section (II), controlling the pressure difference delta P between the upper part and the lower part of the baffling purification section (II) to be 8-10 kPa, and when the pressure difference delta P is higher than the operation range, discharging qualified high-purity graphite powder (with the purity of more than 99.999%) processed in the deep purifier 7 into a blocking material returning device 38 through a discharging pipe at the lower part of the deep purifier 7.

The purification gas used in the purification unit of the present invention is mainly a mixture of an inert gas (mainly argon) and a purification gas (for example, one or more of difluorochloromethane, difluorodichloromethane, trifluorochloromethane, and carbon tetrafluoride). The temperature of the cyclone purifier 2 used in the purification unit is controlled to be 1200-2200 ℃, the gas velocity of the purified gas carrying the graphite powder raw material entering the cyclone purifier 2 is 40-50 m/s, the retention time is 0.5-1.0 h, the operating pressure is-80-140 kPa, the purified gas forms cyclone carrying the graphite powder raw material in the cyclone purifier 2 to purify and produce primary purified graphite powder, remove metals in the graphite powder raw material, the purified gas after primary purification directly enters the air inlet pipes of the circulating pipe 46 at the bottom of the circulating purifier 4 and the side surface of the lower part of the circulating purifier 4, the primary purified graphite powder after cyclone separation is gathered at the lower part of the cyclone purifier 2 and is movably discharged to the primary purified graphite powder bin 3 at the bottom of the cyclone purifier 2, and the primary purified graphite powder is conveyed to the circulating purifier 4 through a bottom pneumatic conveying system; the operation temperature of the circulating purifier 4 is controlled to be 2800-3000 ℃, the operation pressure is-85-145 kPa, the operation gas speed is 3.5-7 m/s, the single circulation residence time is 1-3 min, the total purification time of the primarily purified graphite powder in the circulating purifier 4 is realized by controlling the height of a feed leg discharge port 37 at the lower part of the separator 5, the total purification time is controlled to be 1-1.5 h, and the section is mainly used for reacting high-boiling-point impurities (such as boron, vanadium, molybdenum and the like) in the primarily purified graphite powder with the purified gas to remove and produce the secondarily purified graphite powder; the operation temperature of the deep purifier 7 is also controlled to be 1500-2000 ℃, the operation pressure is-90-150 kPa, the operation gas speed is controlled to be 1.0-2.0 m/s, the residence time of the secondary purified graphite powder in the furnace is controlled to be 10-30 min, and the purified gas separated by the separator 5 enters the bottom of the deep purifier 7 to further react with the secondary purified graphite powder to remove impurities in the graphite powder 2, so that high-temperature qualified high-purity graphite powder (the purity is higher than 99.999%) is produced.

The utility model discloses the gaseous purification that well purification unit finally produced mainly gets into tail gas processing unit and carries out purification treatment and waste heat recovery. Purified gas with the temperature of 1500-2200 ℃ discharged from a purified gas outlet 74 of the deep purifier 7 enters the settling chamber 8, and small granular carbon and the like carried by the purified gas settle in the settling chamber 8; then, the high-temperature purified gas enters a heat exchanger 9 to exchange heat with deoxygenated water and is cooled to 300-350 ℃, and then enters a water washing tower 10; the low-pressure steam with the temperature of 300-400 ℃ and 0.5-1.0 Mpa after heat exchange by the heat exchanger 9 enters the water-cooled wall 145 of the cooler 14 for further heat exchange to generate 3.5-4.0 Mpa and 500-600 ℃ medium-pressure steam for the steam power generation system 15 to generate power; the purified gas at 300-350 ℃ directly contacts water in a reverse-spraying manner in the water washing tower 10 for cooling, and dust, acid gas and the like entering the water enter an alkaline water body, so that the content of harmful substances in the purified gas is effectively reduced; purified gas at 200-250 ℃ washed out from the water scrubber 10 further enters an alkaline liquor spray absorption purification tower 11, and the impurity concentration of the purified gas is greatly reduced; finally, the purified gas after purification treatment is subjected to water-gas separation by a condensation chamber 12 and a gas separator 13 and then recycled to a purification device for reuse. The salt and dust after the washing by circulating water and the alkali washing are settled and then treated regularly, and carbon powder and the like are utilized as auxiliary materials.

The cooling unit of the utility model is mainly used for cooling the high-purity graphite powder (purity is higher than 99.999 percent) produced by the deep purifier 7, the main equipment is the cooler 14 and the air cooling system 16, and the cooling medium is mainly inert gas (mainly argon). The high-temperature high-purity graphite powder generated by the deep purifier 7 enters the cooler 14 through the to-be-cooled high-purity graphite powder outlet 382 of the blocking returning device 38 and the cooler high-purity graphite powder inlet 143. The cooler 14 is operated by fluidization, the cooling medium is inert gas, the cooling medium enters the cooler 14 through an inert gas inlet 23 at the bottom of the cooler 14, and the cooling medium exits the cooler through a cooled inert gas outlet 24. After heat exchange is carried out on the low-pressure steam of 300-400 ℃ by the heat exchanger 9, the low-pressure steam enters the water-cooled wall 145 of the cooler 14 for heat exchange to ensure that the operating temperature of the cooler 14 is controlled below 1200-1500 ℃, the residence time of the high-purity graphite powder in the cooler 14 is controlled to be 0.5-1.0 h, and the operating gas velocity is controlled to be 1.0-1.5 m/s; the high-purity graphite powder product (the purity is higher than 99.999%) discharged from the cooler 14 is cooled to room temperature in the air cooling system 16 and then packaged.

The utility model discloses the produced 3.5 ~ 4.0Mpa of well cooler 14 heat transfer, 500 ~ 600 ℃ middling pressure steam gets into the electricity generation of steam power generation system 15 through the steam outlet 142 of cooler 14 and is used for providing the required electric power of electrical heating for whirl clarifier 2, circulation clarifier 4, degree of depth clarifier 7 and cooler 14, and the produced low pressure steam of steam power generation system 15 then its usefulness.

The utility model discloses the produced tail gas of well purification unit is through gas separation (like membrane separation etc.) again behind the purification treatment inert gas and the separation of purification gas in with the purification gas. Before the purified gas enters the purification unit for purification reaction again, the purified gas lost by graphite powder raw material purification is supplemented at a purified gas adding port 29 (arranged at a purified gas outlet 30) to ensure that the volume of the purified gas required by the purification unit is basically constant; the separated inert gas is used as pneumatic conveying gas of a graphite powder raw material bin 1, pneumatic conveying gas of a bin 3 at the bottom of a cyclone purifier 2 and returning conveying gas of a returning device 6 of a circulating purifier 4. The inert gas used by the cooler 14 is discharged to further cool the pneumatic conveying gas used for the cooling medium of the cooler 14 and the blocking return feeder 38 (the blocking return feeder 38 is basically an L-shaped pipeline, the purified graphite powder returned by the deep purifier is filled in the pipeline, and the graphite powder is conveyed into the cooler by the inert gas on the side surface of the blocking return feeder in a pneumatic mode).

Claims

1. The utility model provides a novel graphite powder is multistage divides accuse degree of depth purification device, its characterized in that, includes purification unit, cooling unit and tail gas processing unit, and wherein, the high-purity graphite powder export (73) of purification unit are connected with cooling unit's high-purity graphite powder entry (143) through blocking returning charge ware (38), and purification gas outlet (74) of purification unit are connected with tail gas processing unit's input.

2. The novel graphite powder multistage separation control deep purification device as claimed in claim 1, wherein the purification unit comprises a cyclone purifier (2), a circulating purifier (4) and a deep purifier (7), a graphite powder raw material and purified gas inlet (33) of the cyclone purifier (2) is connected with an outlet of a graphite powder raw material bin (1), a bin (3) is arranged at the bottom of the cyclone purifier (2), an outlet at the bottom end of the bin (3) is connected with a primary purified graphite powder inlet (41) of the circulating purifier (4), and an exhaust pipe outlet (192) of the cyclone purifier (2) is connected with a purified gas bottom inlet (43) at the bottom end of the circulating purifier (4); the secondary purified graphite powder and the purified gas outlet (45) at the upper part of the circulating purifier (4) are sequentially connected with a secondary purified graphite return port (47) at the lower part of the circulating purifier (4) through a separator (5) and a material return device (6) to form a circulating purification loop; the bottom end of the separator (5) is connected with a secondary purified graphite powder inlet (71) in the middle of the deep purifier (7) through a dipleg (37), a high-purity graphite powder outlet (73) at the bottom end of the deep purifier (7) is connected with a high-purity graphite powder inlet (381) of the blocking return feeder (38), a purified gas air hole (72) of the deep purifier (7) is connected with a gas outlet at the top end of the separator (5), and a purified gas outlet (74) of the deep purifier (7) is connected with the tail gas treatment unit.

3. The novel graphite powder multi-stage separate-control deep purification device as claimed in claim 2, wherein the cyclone purifier (2) comprises a cyclone purifier shell with a closed top end and a cylindrical shape, a coaxial purified gas exhaust pipe (19) is arranged at the middle upper part in the cyclone purifier shell, a bell mouth (191) is arranged at the top end of the purified gas exhaust pipe (19), and an exhaust pipe outlet (192) obliquely led out from the side surface of the cyclone purifier shell is arranged at the lower end of the purified gas exhaust pipe (19); the bottom of the shell of the cyclone purifier is provided with a primary purified graphite powder outlet (36) and a discharging stirring screw (34).

4. The novel graphite powder multistage separation-control deep purification device as claimed in claim 2, wherein the circulation purifier (4) comprises a closed cylindrical circulation purifier shell, a gas distribution pipe (42), a purified gas bottom inlet (43) and a secondary purified graphite return port (47) are respectively arranged in the bottom and at the bottom end of the circulation purifier shell, and a primary purified graphite powder inlet (41) and a purified gas side interface (44) are respectively arranged on the circulation purifier shell above the gas distribution pipe (42) from bottom to top; the top of the shell of the circulation purifier is provided with a secondary purified graphite powder and a purified gas outlet (45).

5. The novel graphite powder multistage separation control depth purification device as claimed in claim 4, wherein the purified gas side interface (44) is arranged on 1-3 circulation pipes (46), a plurality of circulation pipes (46) surround the periphery of the shell of the circulation purifier, and the axial distance between more than two circulation pipes (46) is 0.5-1.5 m; a plurality of air inlet pipes which penetrate into the shell of the circular purifier downwards and obliquely are uniformly connected to the circulating pipe (46) along the circumference, and the included angle alpha between each air inlet pipe and the horizontal direction is 10-15 degrees.

6. The novel graphite powder multistage separation control deep purification device according to claim 2, wherein the deep purifier (7) comprises a V-shaped fluidization section (I), a baffling purification section (II) and a suspension purification section (III) which are sequentially connected from bottom to top, a conical air distribution plate (75) is arranged in the V-shaped fluidization section (I), and an included angle beta between the V-shaped fluidization section (I) and a horizontal plane is 45-60 degrees; air holes are distributed at intervals on the conical air distribution plate (75), the diameter of each air hole is 2-6 mm, and the distance between the air holes is 0.5-1.0 time of the diameter of each air hole; the bottom end of the conical air distribution plate (75) is butted with a high-purity graphite powder outlet (73) arranged at the bottom end of the deep purifier (7); a plurality of purified gas air holes (72) are formed along the periphery of the side surface of the bottom of the deep purifier (7); a plurality of guide cylinders (76) with the same inclination angle as the conical air distribution plate (75) are arranged in the baffling purification section (II), and the guide cylinders (76) are arranged in the baffling purification section (II) in a staggered manner; a secondary purified graphite powder inlet (71) is arranged in the baffling purification section (II) and is connected with the dipleg (37); the diameter of the suspension purification section (III) is larger than that of the baffling purification section (II), and the suspension purification section (III) and the baffling purification section (II) are in transitional connection through a cone; and a purified gas outlet (74) is arranged at the top of the suspension purification section (III) and is connected with the tail gas treatment unit.

7. The novel graphite powder multistage fractional control deep purification device as claimed in claim 2, characterized in that the cooling unit comprises a cooler (14) and an air cooling system (16), wherein a cooled high-purity graphite powder outlet (144) of the cooler (14) is connected with an inlet of the air cooling system (16); a high-purity graphite powder inlet (143) of the cooler (14) is connected with a to-be-cooled high-purity graphite powder outlet (382) of the blocking returning feeder (38); a cooling medium channel inlet (141) of the cooler (14) is connected with a cooling medium outlet of the heat exchanger (9) through a pipeline; the steam outlet (142) of the cooler (14) is connected to a steam power generation system (15).

8. The novel graphite powder multistage separate-control deep purification device as claimed in claim 7, wherein the tail gas treatment unit comprises a settling chamber (8), a heat exchanger (9), a water washing tower (10), an alkaline washing tower (11), a condensing chamber (12) and a gas separator (13) which are sequentially connected through pipelines; wherein the inlet of the settling chamber (8) is connected to the purified gas outlet (74) of the deep purifier (7); a deoxygenated water inlet (28) of the heat exchanger (9) is used for being connected with a cooling medium, and a cooling medium outlet of the heat exchanger (9) is connected with a cooling medium channel inlet (141) of the cooler (14) through a pipeline; the third outlet of the condensing chamber (12) is a condensed water outlet (32); the gas separator (13) is provided with two outlets, namely a purified gas outlet (30) and an inert gas recycling outlet (31), and the purified gas outlet (30) is connected with the graphite powder raw material and the purified gas inlet (33) of the cyclone purifier (2); a purified gas addition port (29) is provided in the purified gas outlet (30).

9. The novel graphite powder multistage separate control deep purification device as claimed in claim 7, wherein the steam outlet (142) of the cooler (14) is connected with a steam power generation system (15), and the steam power generation system (15) is provided with a low-temperature steam outlet (26).