CN113171743B - Integrated equipment for preparing uniform mesophase carbon microspheres by thermal polycondensation method - Google Patents

Integrated equipment for preparing uniform mesophase carbon microspheres by thermal polycondensation method Download PDF

Info

Publication number
CN113171743B
CN113171743B CN202110465232.4A CN202110465232A CN113171743B CN 113171743 B CN113171743 B CN 113171743B CN 202110465232 A CN202110465232 A CN 202110465232A CN 113171743 B CN113171743 B CN 113171743B
Authority
CN
China
Prior art keywords
screen
temperature
layer
stirring paddle
stirring
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202110465232.4A
Other languages
Chinese (zh)
Other versions
CN113171743A (en
Inventor
刘小冬
刘�东
龚鑫
张兰杰
尚亚冰
苏思源
孙畅
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
China University of Petroleum East China
Original Assignee
China University of Petroleum East China
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by China University of Petroleum East China filed Critical China University of Petroleum East China
Priority to CN202110465232.4A priority Critical patent/CN113171743B/en
Publication of CN113171743A publication Critical patent/CN113171743A/en
Application granted granted Critical
Publication of CN113171743B publication Critical patent/CN113171743B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18—Stationary reactors having moving elements inside
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006—Controlling or regulating processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053—Details of the reactor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053—Details of the reactor
    • B01J19/0066—Stirrers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/002—Component parts of these vessels not mentioned in B01J3/004, B01J3/006, B01J3/02 - B01J3/08; Measures taken in conjunction with the process to be carried out, e.g. safety measures
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/02—Feed or outlet devices therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/04—Pressure vessels, e.g. autoclaves
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00—Feed or outlet devices; Feed or outlet control devices
    • B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
    • B01J4/007—Feed or outlet devices as such, e.g. feeding tubes provided with moving parts
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2203/00—Processes utilising sub- or super atmospheric pressure
    • B01J2203/06—High pressure synthesis
    • B01J2203/0605—Composition of the material to be processed
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2204/00—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
    • B01J2204/005—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices the outlet side being of particular interest
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Mixers Of The Rotary Stirring Type (AREA)

Abstract

The invention relates to an integrated device for preparing uniform mesophase carbon microspheres by a direct thermal polycondensation method. In the process of preparing the mesophase globules by thermal polycondensation, the mixed flow created by the specific stirrer can prevent the globules from depositing and melting, and is beneficial to preparing the globules with more uniform particle size distribution; in the high-temperature centrifugation process, the mesophase carbon microspheres in the target particle size range can be obtained by rapid classification separation through a centrifugal screen separator; the control system realizes digital control and optimizes the industrial preparation process of the mesocarbon microbeads. The integrated equipment integrates the processes of preparing, separating, grading, collecting and the like of the mesocarbon microbeads, realizes the optimized configuration of the production processes, has compact and reasonable structure, improves the yield, reduces the energy consumption, greatly reduces the preparation cost of the mesocarbon microbeads and has higher industrial value.

Description

Integrated equipment for preparing uniform mesophase carbon microspheres by thermal polycondensation method
Technical Field
The invention belongs to the technical field of preparing carbon microspheres by a direct thermal polycondensation method, relates to a technology for preparing uniform carbon microspheres by using the direct thermal polycondensation method, and particularly relates to integrated equipment which is beneficial to reducing the fusion of carbon microspheres, shortens the preparation process of mesophase carbon microspheres and realizes the rapid grading preparation of the mesophase carbon microspheres.
Background
The mesocarbon microbeads are optical anisotropic carbon materials with good sphericity, uniform size, high density and ordered lamellar structure, have good self-sintering property, relatively narrow particle size distribution, and excellent characteristics of high stability, high specific surface area, high activity, spherical structure and the like on chemical reagents, can be applied to preparing high-density and high-strength carbon materials, high-performance liquid chromatographic column packing, high-specific surface area active carbon, lithium ion secondary battery electrodes, catalyst carriers and the like, and have high industrial value.
The direct thermal polycondensation method is a common method for preparing the mesocarbon microbeads. The direct thermal polycondensation method has the advantages of simple and easily controlled operation conditions, continuous production and the like, and is widely used in industrial production. However, this method also has disadvantages. In the process of carrying out thermal polycondensation by using the existing stirring rod, because the traditional stirrer adopts a single-layer stirring structure and only has one stirring layer on a transmission rod, some carbon microspheres sink due to self weight and are deposited and fused at the bottom of a kettle body, so that the particle size of the small spheres is not uniform, and the yield of the small spheres is reduced; in addition, the preparation process of the intermediate phase carbon microspheres is complicated at present, and after the intermediate phase carbon microspheres are formed by a direct thermal polycondensation method, the microspheres are separated by a solvent, and the intermediate phase carbon microspheres with different particle sizes can be obtained by performing next cyclone separation.
CN201210009036.7 provides a device for preparing mesocarbon microbeads, wherein a conical settling zone and a material outlet are arranged below a reaction zone of a reaction kettle; by enriching the mesocarbon microbeads in advance, 50% of solvent is saved, and the mesocarbon microbeads are obtained by adopting a cleaning, extracting and extracting mode, so that the separation efficiency is low.
CN201320495107.9 provides a device for separating carbon microspheres from a product containing mesophase carbon microspheres, wherein the container wall of a sealed container is composed of three layers, which are respectively as follows from outside to inside: the device comprises an insulating layer, a conductive layer and a mesh electrode lined on the conductive layer, wherein the bottom of a sealed container is connected with an outlet pipe, the upper part of the sealed container is connected with a product inlet pipe for introducing a product containing the mesophase carbon microspheres with static electricity into the sealed container and a washing solvent inlet pipe for introducing a washing solvent into the sealed container when the mesophase carbon microspheres are washed, and the output end of the electrode of an electrostatic generator which is opposite to the static electricity of the mesophase carbon microsphere product is connected with the mesh electrode. The process is complicated and not suitable for industrial application.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and design integrated equipment which is beneficial to improving the yield of the intermediate phase carbon microspheres prepared by a direct thermal polycondensation method and realizing the rapid grading preparation of the intermediate phase carbon microspheres.
The purpose of the invention is realized by the following technical scheme:
an integrated device for preparing uniform mesophase carbon microspheres by a thermal polycondensation method mainly comprises a high-pressure reaction kettle device provided with a novel stirrer, a high-temperature centrifugal device and a corresponding control system; the high-pressure reaction kettle is communicated with the high-temperature centrifugal device through a control valve;
the novel stirrer is positioned at the middle lower part of the inner cavity of the high-pressure reaction kettle device, adopts a three-layer circulating asymmetric annular stirring structure and comprises a transmission rod and three stirring layers which are unevenly distributed on the transmission rod, and each stirring layer comprises a stirring paddle blade; the blades of the stirring paddle are in an asymmetric elliptical ring-like structure and are connected to the transmission rod; the ring surface of the elliptical ring of the stirring paddle blade is vertical to the horizontal plane and is transversely arranged along the long axis direction; horizontal included angles are formed among the three stirring paddle blades and are positioned at different longitudinal positions; each layer of stirring paddle blade and the transmission rod have different included angles;
preferably, the elliptical ring-like surfaces of the stirring paddle blades are all football-shaped, but the elliptical ring-like surfaces of all the stirring paddle blades are not completely the same in shape; the radius of the section of the ring body of the elliptical ring is 0.5-1.5 cm, and the blades of the stirring paddle have a certain thickness, preferably 0.1-0.3cm.
Preferably, the horizontal included angle between two adjacent stirring paddle blades is 120 degrees, and the vertical interval between two adjacent stirring layers is larger than the minor axis of the elliptical ring and smaller than the major axis of the elliptical ring.
Preferably, the stirring paddle blades in the three stirring layers are all inclined downwards, the inclination degree of the stirring paddle blades is gradually reduced from bottom to top, the included angle between the long axis of the stirring paddle blade in the second layer and the transmission rod is larger than the included angle between the long axis of the stirring paddle blade in the first layer and the transmission rod, and the included angle between the long axis of the stirring paddle blade in the third layer and the transmission rod is larger than the included angle between the long axis of the stirring paddle blade in the second layer and the transmission rod.
Specifically, the included angle between the long axis of the first layer of stirring paddle blades and the transmission rod is 33-37 degrees; the included angle between the long axis of the second layer of the stirring paddle blade and the transmission rod is 45-49 degrees; the included angle between the long axis of the third layer of the stirring paddle blade and the transmission rod is 55-60 degrees.
Preferably, the stirring paddle blade is tangentially welded on the wall of the transmission rod, or the stirring paddle blade and the transmission rod are integrally formed; the intersection point of the long axis of the stirring paddle blade and the transmission rod is preferably 1/4-1/3 of the length of the long axis of the stirring paddle blade.
The high-temperature centrifugal device mainly comprises a high-temperature centrifugal cavity and a centrifugal screen, wherein the centrifugal screen is of a three-layer structure and comprises an inner screen, an outer screen and a collecting net which are sequentially sleeved together from inside to outside, the inner screen, the outer screen and the collecting net are all in an inverted cone shape, and the inner screen and the outer screen form a double-layer screen; the volume of the inner screen is smaller than that of the outer screen, and the aperture of the inner screen is larger than that of the outer screen; the volume of the external screen is smaller than that of the collection net, and the aperture is equal to that of the collection net; the top end of the internal screen is sealed and is communicated with a discharge pipeline of the high-pressure reaction kettle, and the bottom of the internal screen is connected with discharge ports of other products through control valves of external operation switches; the top of the external screen is not sealed, and the bottom of the external screen is directly connected with the axial rotating shaft; the double-layer screen is connected with the same motor rotating shaft, and the rotating speeds of the double-layer screen are the same; and a target product collecting pipeline is arranged at the bottom end of the collecting net.
In the invention, the control system comprises a time control module, a temperature control module, a transmitter, a temperature regulator, a rotating speed regulator, a controller 1 and a controller 2;
the time control module comprises a time display unit and a timer and is used for inputting corresponding reaction time, timing the reaction time of the reaction kettle and controlling the cleaning time after the timing reaction stage is finished;
the temperature control module comprises a temperature display unit and a temperature detection unit, wherein the temperature detection element is positioned on the surface of the reaction kettle, measures the internal temperature of the reaction kettle and transmits the measured temperature to the transmitter;
the transmitter converts the temperature signal from the temperature detection element into a standard electric signal and transmits the standard electric signal to the temperature regulator;
the temperature regulator judges the standard electric signal and regulates and controls the thermocouple;
the rotating speed regulator can input and regulate the rotating speed of the stirring rod;
the controller 1 receives a signal from a timer and controls the on-off of a control valve;
and the controller 2 receives a signal from the controller 1 to close the control valve, controls the motor and adjusts the rotating speed of the centrifugal screen.
The invention relates to an integrated device for preparing mesocarbon microbeads by a thermal polycondensation method, which comprises a control system and a control system, wherein the control system comprises the following steps: the reaction stage of the high-pressure reaction kettle and the high-temperature centrifugal separation stage are controlled by a remote control system;
in the preparation stage of the high-pressure reaction kettle, after the reaction materials are filled, inputting reaction time and reaction temperature in temperature display and time display, and starting a timer when the reaction starts;
in the reaction stage of the high-pressure reaction kettle, a temperature detection element on the outer wall of the reaction kettle monitors the temperature in the reaction kettle in real time, transmits data to a transmitter, converts signals into standard electric signals by the transmitter and transmits the standard electric signals to a temperature regulator, and if the temperature is lower than a set temperature, a thermocouple is regulated to increase the temperature;
when the reaction time reaches the reaction stopping stage, the rotating speed regulator controls the stirring motor to stop stirring; cooling for a period of time, adding a certain amount of washing oil into the reaction kettle through the feeding hole, inputting the reaction temperature in the temperature display again, inputting the cleaning time in the timer, raising the temperature to 150-200 ℃ again, carrying out the cleaning stage, and controlling the timing cleaning time by the timer;
and (2) entering a high-temperature centrifugal separation stage, after cleaning, controlling to open or close a control valve communicating the high-pressure reaction kettle and the high-temperature centrifugal device by the controller 1, enabling the cleaned liquid to flow into an internal screen of the high-temperature centrifugal separation device, after the liquid completely flows out, closing the control valve communicating the high-pressure reaction kettle and the high-temperature centrifugal device by the controller 1, transmitting a signal to the controller 2, and simultaneously inputting the rotating speed of a centrifugal screen according to the separation requirement to perform high-temperature centrifugal separation operation on the mesocarbon microbeads.
In the invention, the stirring paddle blades do not have a conventional symmetrical structure but are in an asymmetrical elliptical ring-like structure, and each layer of stirring paddle blades have a specific structure and a specific installation form to form a three-layer circulation asymmetrical ring-shaped stirring structure. The stirring paddle blades and the transmission shaft are not vertically arranged, but are inclined downwards, three layers have different inclination degrees, the horizontal plane where the intersection point of the long axis of the stirring paddle blades and the transmission rod is located is a transverse interface, each blade is located in an upper stirring area and a lower stirring area, the interior of the whole reactor is divided into six stirring areas from bottom to top, and the transmission rod is used as a longitudinal reference, so that two flow layers with different sizes and different stirring directions are formed in the two adjacent stirring areas; meanwhile, the blades have certain section radius of the ring body, and two flow layers with different sizes and different horizontal stirring directions are formed in the ring body and the inner cavity of the ring; in addition, the blades stir between the flow layer and the flow layer, so that six flow layers with different stirring directions are formed in the horizontal direction and the vertical direction in the reactor respectively. Along with the rotation of the stirring paddle blade driven by the transmission shaft, each flow layer at least circularly flows with the two flow layers, and the fluid generates vortex to stir among the flow layers, so that the stirring is more uniform; in the reaction kettle reaction process, the three layers of stirring paddle blades provide lifting force and downward pressure for the solid microspheres to form different flow layers and stir, so that the stirring efficiency and the space utilization rate are improved, the phenomena of deposition, fusion and uneven particle size of the solid microspheres in the material are greatly reduced, the material waste is reduced, and the reaction preparation efficiency and the conversion rate of the reaction material are improved.
After the mixture of the asphalt mother liquor and the wash oil flows into the internal screen of the high-temperature centrifugal device, the centrifugal screen is driven by the motor and the transmission system to rotate at a high speed, so that the pellets and the wash oil dissolved with isotropic asphalt are quickly separated, and the pellets obtained by separation realize quick classification under the action of the double-layer screen. According to the high-temperature centrifugal device, the aperture of the double-layer screen can be selected and assembled according to the particle size of the target carbon microsphere, the aperture of the inner-layer screen is larger than or equal to the maximum aperture of the target carbon microsphere, so that the carbon microspheres with different particle sizes in the mother liquor are left in the inner-layer screen under the action of centrifugal force, and the target carbon microsphere and the carbon microspheres with smaller particle sizes enter the outer-layer screen through the sieve pores of the inner-layer screen. The aperture of the outer screen is smaller than or equal to the minimum aperture of the target carbon microsphere, so that the carbon microsphere with the particle size smaller than the minimum target in the mother liquor enters the filtrate below through the screen holes of the outer screen, and the carbon microsphere with the target particle size range stays between the inner screen and the outer screen.
Because the rotatory in-process target carbon microsphere of screen cloth can receive corresponding centrifugal force, and inlayer screen cloth top is encapsulated situation, so great carbon microsphere can not climb away along the screen cloth from the inlayer screen cloth, great carbon microsphere will stay inside the inlayer screen cloth, wait for the separation to finish being collected, outer screen cloth upper end is open, under the centrifugal force effect, target carbon microsphere will climb to the top so that fly out along outer screen cloth, so at outer screen cloth outside add the collection net that the one deck is the same with outer screen cloth aperture, be used for collecting target carbon microsphere to collecting pipe.
Compared with the prior art, the invention has the beneficial effects that:
(1) The invention adopts the stirrer with a three-layer circulation asymmetric annular stirring structure, and in the kettle type reaction process, the three-layer stirring paddle blades provide the lifting force and the downward pressure for the materials dissolved in the solvent to form different flow layers and stir the materials, thereby improving the stirring efficiency and the space utilization rate, greatly reducing the material deposition and fusion phenomenon, reducing the material accumulation phenomenon at the bottom layer of the reaction kettle, improving the efficiency of the prepared target product, simultaneously improving the conversion rate of the materials, avoiding the waste of the materials and simplifying the structure of the kettle type reactor to a certain extent.
(2) In the high-temperature centrifugal device designed by the invention, after the mixture of the asphalt mother liquor and the wash oil flows into the screen of the centrifugal separator, the centrifugal screen is driven by the motor and the transmission system to do high-speed rotary motion, so that the small balls and the wash oil dissolved with isotropic asphalt are quickly separated, and simultaneously, the microspheres obtained by separation realize quick classification under the action of the double-layer screen.
(3) The integrated equipment for preparing the uniform mesophase carbon microspheres by the thermal polycondensation method integrates the processes of preparing, separating, grading, collecting and the like of the mesophase carbon microspheres, realizes the optimized configuration of each production process, has compact device, reduces the energy consumption, and greatly reduces the preparation cost of the mesophase carbon microspheres.
(4) The control system designed by the invention realizes digital control by using the temperature control system, the speed control system and the time control system, can input corresponding reaction temperature and time according to production requirements, reduces errors of manual operation by the control system, optimizes the industrial preparation process of the mesocarbon microbeads, and saves human resources by digital control.
Drawings
FIG. 1 is a schematic structural view of an integrated apparatus according to the present invention;
FIG. 2 is a schematic view of the construction of the agitator according to the present invention;
FIG. 3 is a top view of the agitator of the present invention;
fig. 4 is a schematic structural view of three stirring blades of the stirrer.
FIG. 5 is a top view of the inner and outer screens of the present invention.
The device comprises a material inlet 1, a material inlet 2, a motor 3, a cleaning port 4, a thermocouple 5, a pressure gauge 6, a kettle shell 7, a stirrer 8, a material outlet pipeline 9, a control valve 10, a high-temperature centrifugal device 11, a liquid inlet 12, a collection net 13, an internal screen 14, an external screen 15, a motor 16, an axial rotation transmission belt 17, a liquid outlet 18, a target product collection pipeline 19, a material outlet 20 for other products, a high-temperature centrifugal cavity 21 and a support, wherein the material inlet 2 is connected with the material inlet through a pipeline;
a. b and c are intersection points of the long axis of the stirring paddle blade and the transmission rod, r is the section radius of the ring body of the elliptical ring of the stirring paddle blade, d is the thickness of the stirring paddle blade, L1, L2 and L3 are the long axes of the three layers of stirring paddle blades respectively, alpha, beta and gamma are included angles between the long axes of the three layers of stirring paddle blades and the transmission rod respectively, and Z1-Z6 and W1-W6 are different areas formed by the stirring paddle blades.
Detailed Description
The invention is described in detail below with reference to the following figures and detailed description:
as shown in fig. 2-4, the structure of the stirrer 7 is schematically shown; the stirrer adopts a three-layer circular asymmetric annular stirring structure and comprises a transmission rod and three stirring layers which are unevenly arranged on the transmission rod, wherein each stirring layer comprises a stirring paddle blade; the stirring paddle blade is in an asymmetric elliptical ring-like structure and is tangentially welded with the transmission rod or integrally formed with the transmission rod, and the intersection point a (b/c) of the long axis L of the stirring paddle blade and the transmission rod 1 is 1/4-1/3 of the length of the long axis of the stirring paddle blade;
the elliptical ring surfaces of the stirring paddle blades are all football-shaped, but the elliptical ring surfaces of all the stirring paddle blades are not completely the same in shape; the radius r of the section of the ring body of the elliptical ring is 0.5-1.5 cm, and the thickness d of the blade of the stirring paddle is 0.1-0.3cm;
the ring surface of the elliptical ring of the stirring paddle blade is vertical to the horizontal plane and is transversely arranged along the long axis direction; horizontal included angles are formed among the three stirring paddle blades and are positioned at different longitudinal positions; the horizontal included angle between two adjacent stirring paddle blades is 120 degrees, and the vertical interval between two adjacent stirring layers is greater than the short axis of the elliptical ring and less than the long axis of the elliptical ring; each layer of stirring paddle blade and the transmission rod have different included angles; the stirring paddle blades in the three stirring layers are all inclined downwards, from bottom to top, and the long axis L of the first layer of stirring paddle blade 1 The included angle alpha between the stirring paddle blade and the transmission rod 1 is 33-37 degrees, so that an upper area Z and a lower area Z are formed by taking the horizontal plane where the connecting point a of the long shaft of the stirring paddle blade and the transmission rod is positioned as the horizontal reference 1 And Z 2 Ensure that two stirring streams with different sizes are formed in the two areasThe flow layers with different stirring directions are formed, the blades have certain radius of the section of the ring body, and two flow layers W1 and W2 with different sizes and different horizontal stirring directions are formed on the section of the ring body and the inner cavity of the ring; the blades also stir between the flow layers. Major axis L of second layer stirring paddle blade 2 The included angle beta between the stirring paddle and the transmission rod is 45-49 degrees, and the long axis L of the third layer of stirring paddle blades 3 The included angle gamma between the blade and the transmission rod is 55-60 degrees, the same principle is adopted, six flow layers with different directions and sizes are respectively formed in the horizontal direction and the vertical direction, three asymmetric elliptical ring-like structure blades are continuously stirred between the flow layers, and because the angle of each flow layer is different, each flow layer at least flows circularly with two flow layers, so that the stirring between the flow layers is ensured when the blades are stirred, the fluid per se also generates vortex to stir the flow layers, the stirring is more uniform, and the distribution of materials is more uniform during the reaction.
In a reaction kettle in practical application, the working position of the stirrer is similar to that of a common stirring rod, materials and solvents are stirred in the working process of the reaction kettle, six mutually intersected flow layers are generated when solid-liquid mixing is stirred by utilizing a designed specific structure, and when various flow layers are stirred in a convection mode (mixed flow at the moment), regular circulation stirring is carried out on all space areas because the stirring blades also have thicknesses, so that the uniformity of solid-liquid in the whole space is ensured, the stirring is more uniform, and powerful environmental conditions are provided for reaction.
The high-temperature centrifugal device mainly comprises a high-temperature centrifugal cavity and a centrifugal screen, wherein the centrifugal screen is of a three-layer structure and comprises an inner screen 13, an outer screen 14 and a collection net 12 which are sequentially sleeved together from inside to outside, the inner screen 13, the outer screen 14 and the collection net 12 are all in inverted cone shapes, and the inner screen 13 and the outer screen 14 form a double-layer screen; the inner screen 13 has a smaller volume and a larger aperture than the outer screen 14; the outer screen 14 has a volume smaller than that of the collection screen 12 and a pore size equal to that of the collection screen; the top end of the internal screen 13 is sealed and is communicated with a discharge pipeline 8 of the high-pressure reaction kettle, and the bottom of the internal screen is connected with other product discharge ports 19 through control valves; the top of the outer screen 14 is not sealed, and the bottom is directly connected with the axial rotating shaft; the double-layer screen is connected with the same motor rotating shaft, and the rotating speeds of the double-layer screen are the same; the bottom end of the collection net has a destination product collection conduit 18.
Example 1
Preparing carbon microspheres by a direct thermal polycondensation method: weighing a certain amount of raw oil and carbon black (5%) in a certain mass proportion, uniformly mixing, ultrasonically dispersing for 1h, pouring the mixture into the kettle-type reactor, replacing nitrogen for 3 times, and filling the pressure in the kettle to 3MPa; setting the temperature to 430 ℃, setting the rotating speed of the stirrer 7 to 400r/min by a rotating speed regulator, increasing the reaction temperature to a certain temperature (430 ℃) at 5 ℃/min in the temperature setting for reacting for a certain time, displaying the time and setting the reaction time to 8h, and maintaining the pressure in the kettle to be 3MPa by regulating a deflation valve in the reaction process; in the reaction process, the temperature in the reaction kettle is monitored in real time by a temperature detection element on the surface of the kettle, a temperature signal is transmitted to a transmitter, the transmitter converts the temperature signal into a standard transmission signal and transmits the standard transmission signal to a regulator for regulation, and if the temperature in the kettle is lower than a set temperature, the regulator controls a heating galvanic couple 4 to enable the temperature in the kettle to rise; after the set reaction time is over, the rotation speed regulator receives a signal from time display, stops stirring, resets the display temperature to 150 ℃, naturally cools to reduce the temperature in the kettle to the set temperature for cleaning the carbon microspheres, adds a certain amount of washing oil into the reaction kettle through the feed inlet, resets the separation rotation speed at the rotation speed regulator to 300r/min, inputs the reaction temperature in the temperature display again, increases the temperature to 150-200 ℃, inputs the cleaning time at the timer for 1h, carries out a cleaning stage, and controls the timing of the cleaning time by the timer;
entering a high-temperature centrifugal separation stage, after cleaning, controlling to open or close a control valve 9 communicating the high-pressure reaction kettle and the high-temperature centrifugal device by a controller 1, enabling the cleaned liquid to flow into an internal screen 13 of the high-temperature centrifugal separation device, after the liquid completely flows out, closing the control valve 9 communicating the high-pressure reaction kettle and the high-temperature centrifugal device by the controller 1, transmitting a signal to the controller 2, inputting a rotating speed of the centrifugal screen into a rotating speed regulator according to the separation requirement, controlling the rotating speed by a motor 15, controlling the centrifugal time to be 5-7min, controlling the centrifugal temperature to be 150-200 ℃, and carrying out the high-temperature centrifugal separation operation of the mesocarbon microbeads.
After the mixture of the asphalt mother liquor and the washing oil flows into an inner screen 13 of the high-temperature centrifugal device, the centrifugal screen is driven by a motor and a transmission system to do high-speed rotary motion, so that the pellets and the washing oil dissolved with isotropic asphalt are quickly separated, the aperture of an outer screen 14 is smaller than or equal to the minimum aperture of a target carbon microsphere, the carbon microsphere with the particle size smaller than the minimum target in the mother liquor enters a filtrate below through a sieve hole of the outer screen 14, and the carbon microsphere with the target particle size range stays between the inner screen 13 and the outer screen 14; in this embodiment, the outer screen 14 has a pore size of 10 μm, and the inner screen 13 has a pore size of 20 μm.
Because the rotatory in-process target carbon microsphere of screen cloth can receive corresponding centrifugal force, and inlayer screen cloth top is encapsulated situation, so great carbon microsphere can not climb away along the screen cloth from the inlayer screen cloth, great carbon microsphere will stay inside the inlayer screen cloth, wait for the separation to finish being collected, collect from other product discharge gates 19, outer screen cloth upper end is open, under the centrifugal force effect, target carbon microsphere will climb to the top so that fly out along outer screen cloth, so add the collection net that the one deck is the same with outer screen cloth aperture in outer screen cloth outside, be used for collecting target carbon microsphere to purpose product collecting tube 18.
The mesocarbon microbeads with uniform size and good sphericity are prepared in the embodiment, the particle size distribution of the microbeads is concentrated at 10-20 microns, and the yield is 47-49%.
Comparative example 1
The stirrer provided by the invention is replaced by a conventional flap blade type stirrer in the reaction kettle, otherwise, as in example 1, the fused mesophase microspheres are stacked at the bottom of the reaction kettle, the separated mesophase carbon microspheres have uneven sizes and general sphericity, and the yield of the spherules with particle size distribution concentrated between 10 and 20 microns is 20.6 to 25 percent.
Comparative example 2
The reactor and the stirrer in the embodiment 1 are adopted for thermal polycondensation to prepare the mesocarbon microbeads, a centrifugal screen with a three-layer structure is not arranged, and the extraction ratio of wash oil is 2:1, the extraction temperature is 170 ℃, the extraction time is about 2 hours, and the carbon microspheres with the particle size of 1-40 microns are obtained after cleaning, the yield is 30-35%, wherein the carbon microspheres with the particle size of 10-20 microns account for about 20.6%. Because no proper means is available for separating the pellets in the next step, only the part of pellets of 1-40 microns can be carbonized, and then the battery is prepared, so that the charging and discharging are unstable due to the difference of the particle sizes of the pellets, and the electrochemical performance is not perfect.

Claims (6)

1. An integrated device for preparing mesocarbon microbeads by a thermal polycondensation method is characterized by mainly comprising a high-pressure reaction kettle with a novel stirrer, a high-temperature centrifugal device and a corresponding control system; the high-pressure reaction kettle is communicated with the high-temperature centrifugal device through a control valve;
the novel stirrer is positioned at the middle lower part of the inner cavity of the high-pressure reaction kettle device, adopts a three-layer circulating asymmetric annular stirring structure and comprises a transmission rod and three stirring layers which are unevenly distributed on the transmission rod, and each stirring layer comprises a stirring paddle blade; the stirring paddle blade is in an asymmetric elliptical ring-like structure and is connected to the transmission rod; the elliptical ring surfaces of the stirring paddle blades are all football-shaped, but the elliptical ring surfaces of all the stirring paddle blades are not completely the same in shape; the section radius of the ring body of the elliptical ring is 0.5-1.5 cm, and the blades of the stirring paddle have a certain thickness of 0.1-0.3cm; the ring surface of the elliptical ring of the stirring paddle blade is vertical to the horizontal plane and is transversely arranged along the long axis direction; the three stirring paddle blades have horizontal included angles of 120 degrees and are positioned at different longitudinal positions; the vertical interval between two adjacent stirring layers is greater than the minor axis of the elliptical-like ring and less than the major axis of the elliptical-like ring; the intersection point of the long axis of the stirring paddle blade and the transmission rod is at 1/4~1/3 of the length of the long axis of the stirring paddle blade;
the stirring paddle blades in the three stirring layers are all inclined downwards, the inclination degree of the stirring paddle blades is gradually reduced from bottom to top, and the included angle between the long axis of the first layer of stirring paddle blades and the transmission rod is 33-37 degrees; the included angle between the long axis of the second layer of the stirring paddle blade and the transmission rod is 45-49 degrees; the included angle between the long axis of the third layer of the stirring paddle blade and the transmission rod is 55-60 degrees;
the high-temperature centrifugal device mainly comprises a high-temperature centrifugal cavity and a centrifugal screen, wherein the centrifugal screen is of a three-layer structure and comprises an inner screen, an outer screen and a collection net which are sequentially sleeved together from inside to outside, the inner screen, the outer screen and the collection net are all in inverted cone shapes, and the inner screen and the outer screen form a double-layer screen; the volume of the inner screen is smaller than that of the outer screen, and the aperture of the inner screen is larger than that of the outer screen; the volume of the external screen is smaller than that of the collection net, and the aperture is equal to that of the collection net; the top end of the internal screen is sealed and is communicated with a discharge pipeline of the high-pressure reaction kettle, and the bottom of the internal screen is connected with discharge ports of other products through a control valve of an external operating switch; the top of the external screen is not sealed, and the bottom of the external screen is directly connected with the axial rotating shaft; the double-layer screen is connected with the same motor rotating shaft, and the rotating speeds of the double-layer screen are the same; a target product collecting pipeline is arranged at the bottom end of the collecting net;
the aperture of the double-layer screen is selected and assembled according to the particle size of the target carbon microsphere, the aperture of the inner-layer screen is larger than or equal to the maximum aperture of the target carbon microsphere, so that the carbon microspheres with larger particle sizes in the mother liquor are left in the inner-layer screen under the action of centrifugal force, and the target carbon microsphere and the carbon microspheres with smaller particle sizes enter the outer-layer screen through the sieve pores of the inner-layer screen; the aperture of the outer layer screen is smaller than or equal to the minimum aperture of the target carbon microsphere, so that the carbon microsphere with the particle size smaller than the minimum target in the mother liquor enters the filtrate below through the sieve pores of the outer layer screen, and the carbon microsphere with the target particle size range stays between the inner layer screen and the outer layer screen;
the control system comprises a time control module, a temperature control module, a transmitter, a temperature regulator, a rotating speed regulator, a controller 1 and a controller 2.
2. The integrated equipment for preparing mesocarbon microbeads through thermal polycondensation according to claim 1, wherein the stirring paddle blades are tangentially welded on the wall of the transmission rod or are integrally formed with the transmission rod.
3. The integrated equipment for preparing mesocarbon microbeads through thermal polycondensation according to claim 1, wherein the outer layer of screen has a pore size of 10 microns and the inner layer of screen has a pore size of 20 microns.
4. The integrated equipment for preparing the mesocarbon microbeads through the thermal polycondensation method according to claim 1, wherein the time control module comprises a time display unit and a timer and is used for inputting corresponding reaction time, timing the reaction time of the reaction kettle and controlling the cleaning time after the timing reaction stage is finished;
the temperature control module comprises a temperature display unit and a temperature detection unit, wherein the temperature detection element is positioned on the surface of the reaction kettle, measures the internal temperature of the reaction kettle and transmits the measured temperature to the transmitter;
the transmitter converts the temperature signal from the temperature detection unit into a standard electric signal and transmits the standard electric signal to the temperature regulator;
the temperature regulator judges the standard electric signal and regulates and controls the thermocouple;
the rotating speed regulator can input and regulate the rotating speed of the stirring rod;
the controller 1 receives a signal from a timer and controls the on-off of a control valve;
and the controller 2 receives a signal from the controller 1 to close the control valve, controls the motor and adjusts the rotating speed of the centrifugal screen.
5. The integrated equipment for preparing the mesocarbon microbeads through the thermal polycondensation method according to claim 4, wherein the operation process of the control system is as follows: the reaction stage and the high-temperature centrifugal separation stage of the high-pressure reaction kettle are controlled by a remote control system;
in the preparation stage of the high-pressure reaction kettle, after the reaction materials are filled, inputting reaction time and reaction temperature in temperature display and time display, and starting a timer when the reaction starts;
in the reaction stage of the high-pressure reaction kettle, a temperature detection element on the outer wall of the reaction kettle monitors the temperature in the reaction kettle in real time, transmits data to a transmitter, and converts a signal into a standard electric signal by the transmitter and transmits the standard electric signal to a temperature regulator;
when the reaction time reaches the reaction stopping stage, the rotating speed regulator controls the stirring motor to stop stirring; cooling for a period of time, adding a certain amount of washing oil into the reaction kettle through the feeding hole, inputting the reaction temperature in the temperature display again, inputting the cleaning time in the timer, raising the temperature to 150-200 ℃ again, carrying out the cleaning stage, and controlling the timing cleaning time by the timer;
and (2) entering a high-temperature centrifugal separation stage, after cleaning, controlling to open or close a control valve for communicating the high-pressure reaction kettle with the high-temperature centrifugal device by the controller 1, enabling the cleaned liquid to flow into an internal screen of the high-temperature centrifugal separation device, after the liquid completely flows out, closing the control valve for communicating the high-pressure reaction kettle with the high-temperature centrifugal device by the controller 1, transmitting a signal to the controller 2, and simultaneously inputting the rotating speed of a centrifugal screen according to the separation requirement to perform the high-temperature centrifugal separation operation of the mesocarbon microbeads.
6. The integrated equipment for preparing the mesocarbon microbeads through the thermal polycondensation method according to claim 1, wherein the particle size distribution of the mesocarbon microbeads prepared by the integrated equipment is concentrated in 10-20 microns, and the yield is 47-49%.
CN202110465232.4A 2021-04-28 2021-04-28 Integrated equipment for preparing uniform mesophase carbon microspheres by thermal polycondensation method Active CN113171743B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110465232.4A CN113171743B (en) 2021-04-28 2021-04-28 Integrated equipment for preparing uniform mesophase carbon microspheres by thermal polycondensation method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110465232.4A CN113171743B (en) 2021-04-28 2021-04-28 Integrated equipment for preparing uniform mesophase carbon microspheres by thermal polycondensation method

Publications (2)

Publication Number Publication Date
CN113171743A CN113171743A (en) 2021-07-27
CN113171743B true CN113171743B (en) 2022-10-25

Family

ID=76927008

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110465232.4A Active CN113171743B (en) 2021-04-28 2021-04-28 Integrated equipment for preparing uniform mesophase carbon microspheres by thermal polycondensation method

Country Status (1)

Country Link
CN (1) CN113171743B (en)

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA2864735A1 (en) * 2012-02-17 2013-08-22 Run4 Pty Ltd Drive assembly and exercise apparatus including a drive assembly
CN205435553U (en) * 2015-12-29 2016-08-10 张玮 Medical mixer with reducing mechanism

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101227796B1 (en) * 2011-01-11 2013-01-29 경기대학교 산학협력단 Carbon sphere-catalytic oxide nano composites for lithium-air secondary battery and manufacturing method of the same
CN202410273U (en) * 2011-08-27 2012-09-05 天津市贝特瑞新能源材料有限责任公司 Washing and filtering integrated device used in preparation of mesocarbon microbeads
CN203400680U (en) * 2013-07-30 2014-01-22 南京格洛特环境工程有限公司 Stirrer for chemical solution
CN110364730A (en) * 2018-03-26 2019-10-22 北京化工大学 A kind of preparation method of mesophase pitch carbon microspheres
CN210252127U (en) * 2019-06-05 2020-04-07 南京恒桥化学技术材料有限公司 Novel photoinitiator stirring reaction kettle

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA2864735A1 (en) * 2012-02-17 2013-08-22 Run4 Pty Ltd Drive assembly and exercise apparatus including a drive assembly
CN205435553U (en) * 2015-12-29 2016-08-10 张玮 Medical mixer with reducing mechanism

Also Published As

Publication number Publication date
CN113171743A (en) 2021-07-27

Similar Documents

Publication Publication Date Title
CN101744722B (en) Dripping pill production line
CN106345375B (en) A kind of common loop reactor simultaneous with reaction and separation function
CN202725165U (en) Particle crystallization reaction system for preparation of lithium battery material precursor
CN105396650A (en) Screen-free type intelligent nanometer grinding system
CN113171743B (en) Integrated equipment for preparing uniform mesophase carbon microspheres by thermal polycondensation method
CN108554335B (en) Mixed fluid stirring mechanism and tubular reactor
CN107895791A (en) The classification handling process of nickel-cobalt-manganese ternary material precursor
CN216935640U (en) Stirring tank for producing high polymer material
CN215353891U (en) Smashing device for silicon dioxide film material for ultra-dense vacuum coating
CN208406149U (en) A kind of device of separating durene by freezing crystallization
CN204996494U (en) No screen cloth formula intelligence nanometer system of grinding
CN201350218Y (en) Dripping pill production line
CN207327347U (en) Plastics-production agitating device
CN217829614U (en) Be used for high-efficient mixing arrangement of artificial graphite anode material
CN219279505U (en) Air inlet structure of polysilicon reduction furnace
CN202962569U (en) Vertical type reinforced polysaccharide high polymer modifying and stirring ball-milling reactor
CN202876777U (en) Novel esterification pre-reactor
CN202410655U (en) Mist type conical reactor
CN104707541A (en) Sectional type cyclone reaction kettle for homogeneous reaction
CN111715418B (en) Composite grading equipment
CN103908810B (en) A kind of yellow phosphorus sewage water treatment method and device thereof
CN102060651B (en) Method and device for combining and separating mixed xylene slurry
CN211636446U (en) Gas distributor and anthraquinone hydrogenation slurry bed reactor
CN112251332B (en) Anti-crusting fermentation device
CN212504611U (en) Straight cylinder type light-burned magnesium oxide suspension roasting device

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant