CN109179367A - A kind of thermal polycondensation process prepares the method and system of carbonaceous mesophase spherules - Google Patents
A kind of thermal polycondensation process prepares the method and system of carbonaceous mesophase spherules Download PDFInfo
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- CN109179367A CN109179367A CN201811051791.5A CN201811051791A CN109179367A CN 109179367 A CN109179367 A CN 109179367A CN 201811051791 A CN201811051791 A CN 201811051791A CN 109179367 A CN109179367 A CN 109179367A
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- C01—INORGANIC CHEMISTRY
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Abstract
The invention belongs to carbon materials preparation method for material and equipment technical fields, and in particular to a kind of thermal polycondensation process prepares the method and system of carbonaceous mesophase spherules.The present invention controls formation and the precipitation process of mesocarbon microspheres by substep, in conjunction with high temperature centrifugal filtration, solve the problems such as existing pyrocondensation polymerizing technology partial size is not easy to control, separation is difficult, yield is low, the pollution to environment is reduced by closed-loop control, technical process is easily realized, and no pollution to the environment, the mesocarbon microspheres grain good sphericity of preparation, diameter uniform, controllable, narrowly distributing, high income.
Description
Technical field
The invention belongs to carbon materials preparation method for material and equipment technical fields, and in particular to a kind of thermal polycondensation process preparation interphase
The method and system of carbosphere.
Background technique
When pitch class compound is heat-treated, thermal polycondensation reaction generation, which occurs, has anisotropic mesophasespherule,
Mesophase ball separates the nano-level sphere carbon material to be formed from pitch precursor and is known as mesocarbon microspheres
(Mesocarbon microbeads, abbreviation MCMB).
Mesocarbon microspheres is a kind of new function material, and inside is the synusia molecule laminated construction of similar graphite, is had
Excellent physics and chemical property, such as good chemical stability, thermal stability, self sintering, high electrical and thermal conductivity are
Prepare non-bonding-agent high-density degree high-strength carbon material, active carbon with superhigh specific surface area, serondary lithium battery negative electrode material, high-efficient liquid phase color
The quality raw materials for composing the high performance Carbon Materials such as filler, catalyst carrier, possess wide application and prospect.
The preparation method of mesocarbon microspheres is mainly thermal polycondensation process and emulsion process at present.Emulsion process procedure complexity,
The carbon microspheres prepared are fusible, and cure treatment must be passed through before charing, and production cost is higher.Interphase in thermal polycondensation process
The formation of carbon microspheres can be divided into three steps: being nucleated, grow up, melting simultaneously, to obtain uniform particle sizes and the good MCMB of monodispersity, needing
Promote the nucleation of MCMB and limit it to melt simultaneously, the former needs to generate a large amount of intermediate phase molecule, and the latter needs to control interphase
Development, at present for coordinate nucleation and melt and contradiction, mostly in process system be added carbon black, silica gel, graphite intercalation compound,
The additives such as ferrocene.On the whole, thermal polycondensation method there is problems: it is more difficult 1. to separate pure MCMB；2. yield
It is lower, it is usually no more than 20%；3. particle diameter distribution is wider；4. remaining additive influences the subsequent processing of MCMB；5. polluting ring
Border.These problems limit its application prospect.
Summary of the invention
The purpose of the present invention is in view of the above technical problems, provide a kind of method that thermal polycondensation process prepares carbonaceous mesophase spherules
And system.
In order to solve the above technical problems, the technical solution adopted by the present invention are as follows:
A kind of method that thermal polycondensation process prepares carbonaceous mesophase spherules, includes the following steps:
1) material asphalt is put into asphalt stock slot, is warming up to 150-200 DEG C, and constant temperature to pitch liquefies, and obtains liquid phase pitch
Raw material；
2) input of liquid phase asphalt stock has the reaction kettle of blender, and inert gas shielding is warming up to 400-450 DEG C, pressure
Power 0.5-0.7MPa, mixing speed 200-400r/min, constant temperature thermal polycondensation 5-7h obtain the mother liquor rich in mesophasespherule and drip
It is green；
3) washing oil that is previously implanted of subsider with blender, constant temperature into that will contain after 100-150 DEG C while stirring
Between mutually spherular mother liquor pitch from reaction kettle input subsider, mixing speed 200-400r/min, constant temperature to 100-150 DEG C,
Residence time 1-5h, mesophasespherule settle out to form carbonaceous mesophase spherules, obtain the sedimentation containing carbonaceous mesophase spherules
Liquid；
4) the sedimentation liquid pump containing carbonaceous mesophase spherules is delivered to the sedimentation liquid head tank with blender, mixing speed
200-400r/min, constant temperature is to 100-120 DEG C；
5) sedimentation liquid after constant temperature is delivered to centrifuge centrifuge separation from sedimentation liquid head tank, and the mesocarbon isolated is micro-
Ball is first cleaned with toluene in centrifuge, is then cleaned again with washing oil, centrifuge speed 8000-15000r/min；
6) carbonaceous mesophase spherules after cleaning enter tray drier by charger and dry, and 350-420 DEG C of drying temperature,
Drying time 15-30min；
7) carbonaceous mesophase spherules after drying enter blade cooler and are cooled to room temperature, and it is micro- to be packaged to be finished product mesocarbon
Ball.Material asphalt liquefies in advance is conducive to the uniform progress of thermal polycondensation reaction, realizes that the closing of technical process carries out, reduces technique
Pollution of the process to environment.Condensing temperature is more than 200 DEG C, and flue gas generation is more, and temperature is lower than 150 DEG C, and liquefying speed is slow, unfavorable
Obtain uniform heat polycondensation of raw materials.Temperature of reaction kettle is more than 450 DEG C, and reaction speed is too fast, easily forms body interphase, temperature of reaction kettle
Lower than 400 DEG C, interphase forms difficulty, is difficult to obtain the mesocarbon microspheres of uniform particle sizes.The stirring of reaction kettle and stirred tank
Speed is more than 400r/min, and mesophasespherule easily deforms under shearing force, cannot get the good product of sphericity,
Mixing speed is lower than 200r/min, and mesophasespherule easily melts simultaneously.Subsider temperature control is conducive to control at 100-150 DEG C
The speed to form mesocarbon microspheres is precipitated in mesophasespherule, obtains the product of uniform particle sizes.Sedimentation liquid head tank stirring speed
200-400r/min is spent, temperature control is conducive to mesocarbon microspheres and is dispersed in sedimentation liquid, be convenient for 100-120 DEG C
It is centrifugated out mesocarbon microspheres.Drying temperature is more than 420 DEG C, and mesocarbon microspheres can occur to aoxidize and melt, and is lower than 350
DEG C, washing oil cannot completely remove.
Further, material asphalt is coal tar pitch in the step 1), and softening point is 75-80 DEG C, quinoline insolubles≤4%.
Quinoline insolubles are more than 4%, and influence intermediate phase molecule piles up process, easily causes mesophasespherule existing defects.
Further, the amount that subsider washing oil is previously implanted in the step 3) is the 1/4-1/2 of mother liquor pitch volume.It washes
The amount of oil is more than the 1/2 of mother liquor pitch volume, and mesophasespherule sedimentation is too fast, is easily melted simultaneously, and the amount of washing oil is less than mother liquor
The 1/4 of pitch volume, mesophasespherule sedimentation is difficult, is difficult to obtain the product of uniform particle sizes.
Further, speed of the mother liquor pitch in the step 3) containing mesophasespherule from reaction kettle input subsider
It spends control settlement bath temperature and rises and be no more than 10 DEG C/min.Mesocarbon microspheres speed of separating out is controlled, help to obtain uniform particle sizes'
Spherula.
Further, the specific method being centrifugated in the step 5) is high temperature centrifugal filtration, and centrifugal filtration temperature is
100-120℃.Mesocarbon microspheres is solid phase at this time, and sedimentation liquid is the lesser liquid phase of viscosity, and it is micro- to efficiently separate out intermediate-phase carbon
Ball.
Further, the toluene of cleaning carbonaceous mesophase spherules and the temperature of washing oil are 30-50 DEG C in the step 5), toluene
Cleaning 1-2 times, each dosage are 1-2 times of carbonaceous mesophase spherules quality, and washing oil cleans 2-4 times, and each dosage is mesocarbon
1-2 times of microspheres quality.Economy easily cleans up the liquid on mesocarbon microspheres surface.
Further, the washing oil after the liquid being centrifugated out in the step 5) and cleaning is recycled to mother liquor tank, toluene
Into solvent recovery slot, recycled after separation.Reduce production cost.
Further, the asphalt stock slot, reaction kettle, subsider, sedimentation liquid head tank, centrifuge, tray drier
The flue gas of generation absorbs reuse with washing oil after Venturi tube, and residual gas is through burning disposal.Part in one side recovered flue gas
Component is used as washing oil, further decreases production cost, another aspect tail gas avoids pollution environment through burning disposal.
A kind of system that thermal polycondensation process prepares carbonaceous mesophase spherules, including asphalt stock slot, reaction kettle, subsider, sedimentation
Liquid head tank, washing oil head tank, centrifuge, mother liquor tank, washing oil slot, solvent tank, solvent head tank, solvent recovery slot, driving
Conveying device, charger, tray drier, paddle cooler and packing apparatus,
The feed inlet that the discharge port of the asphalt stock slot passes through pipeline and reaction kettle equipped with pump connects, and reaction kettle goes out
Material mouth is connected by the mother liquor bitumen feed mouth of pipeline and subsider, and the discharge port of subsider is by being equipped with the pipeline of oil pump and sinking
The feed inlet of descending liquid head tank connects, and the discharge port of sedimentation liquid head tank is connected by the sedimentation liquid feed inlet of pipeline and centrifuge
It connects, threeway is arranged in the discharge port of washing oil head tank, and a discharge end is connected by the washing oil feed inlet of pipeline and subsider, separately
One discharge end is connected by the washing oil feed inlet of pipeline and centrifuge, and the discharge port of washing oil slot is high-order by pipeline and washing oil
The feed inlet of slot connects, and the discharge port of solvent tank is connect by pipeline with the feed inlet of solvent head tank, solvent head tank
Discharge port is connected by the solvent feed mouth of pipeline and centrifuge, centrifuge cleaning agent outlet setting threeway, a discharge end
It being connected by the feed inlet of pipeline and mother liquor tank, another discharge end is connect by pipeline with the feed inlet of solvent recovery slot,
The side of centrifuge solid phase discharge port is arranged in driving conveying device, and the feed inlet setting of charger is in driving conveying device blanking
The underface of mouth, the discharge port of charger and the feed inlet of tray drier connect, and the discharge port and paddle of tray drier are cold
But packing apparatus is arranged in the feed inlet connection of machine, the discharge outlet of paddle cooler.Closed-loop control is realized in production procedure, is not polluted
Environment.
Further, the system for preparing carbonaceous mesophase spherules further includes smoke depressant systems, and smoke depressant systems are successively by Wen
Pipe, washing oil absorb slot and connect composition with incineration system, and the reaction kettle, subsider, sedimentation liquid head tank, centrifuge and disc type are dry
The smoke outlet of dry machine is connected by the Venturi tube smoke inlet of pipeline and smoke depressant systems.Constituent part in one side recovered flue gas is used
Make washing oil, further decrease production cost, another aspect tail gas avoids pollution environment through burning disposal.
The invention adopts the above technical scheme, and formation and the precipitation process of mesocarbon microspheres are controlled by substep, in conjunction with
High temperature centrifugal filtration solves the problems such as existing pyrocondensation polymerizing technology partial size is not easy to control, separation is difficult, yield is low, passes through closed loop control
System reduces the pollution to environment, and technical process is easily realized, and no pollution to the environment, mesocarbon microspheres grain such as Fig. 1, the figure of preparation
Shown in 2 and Fig. 3, good sphericity, diameter uniform, controllable, narrowly distributing, high income.
Detailed description of the invention
Fig. 1-2 is the scanning electron microscope (SEM) photograph of the carbonaceous mesophase spherules of the bright preparation of we；
Fig. 3 is the particle diameter distribution analysis chart of the carbonaceous mesophase spherules of the bright preparation of we；
Fig. 4 is the structural schematic diagram for the system that the present invention prepares carbonaceous mesophase spherules.
Specific embodiment
Embodiment 1
The method that one of the present embodiment thermal polycondensation process prepares carbonaceous mesophase spherules, includes the following steps:
1) raw material coal tar pitch is put into asphalt stock slot, is warming up to 150 DEG C, and constant temperature to pitch liquefies, and it is former to obtain liquid phase pitch
Material；The coal tar pitch softening point is 75-80 DEG C, quinoline insolubles≤4%.
2) input of liquid phase asphalt stock has the reaction kettle of blender, and inert gas shielding is warming up to 400 DEG C, pressure
0.5MPa, mixing speed 200r/min, constant temperature thermal polycondensation 7h obtain the mother liquor pitch rich in mesophasespherule；
3) washing oil that the subsider with blender is previously implanted, the amount for being previously implanted subsider washing oil is mother liquor pitch body
Mother liquor pitch containing mesophasespherule is inputted subsider from reaction kettle while stirring to after 100 DEG C by long-pending 1/4, constant temperature,
Input speed control settlement bath temperature rise be no more than 10 DEG C/min, mixing speed 200r/min, constant temperature to 100 DEG C, residence time 5h,
Mesophasespherule settles out to form carbonaceous mesophase spherules, obtains the sedimentation liquid containing carbonaceous mesophase spherules；
4) the sedimentation liquid pump containing carbonaceous mesophase spherules is delivered to the sedimentation liquid head tank with blender, mixing speed
200r/min, constant temperature is to 100 DEG C；
5) sedimentation liquid after constant temperature is delivered to centrifuge from sedimentation liquid head tank and carries out high temperature centrifugal filtration separation, is centrifuged
Filtering temperature is 100 DEG C, and the carbonaceous mesophase spherules isolated first carry out cleaning 1 time with toluene in centrifuge；Then washing oil is used again
Cleaning 2 times is carried out, toluene and each dosage of washing oil are 1 times of carbonaceous mesophase spherules quality, clean the toluene of carbonaceous mesophase spherules
Temperature with washing oil is 30 DEG C, centrifuge speed 8000r/min, and the washing oil after the liquid being centrifugated out and cleaning is recycled to mother
Liquid bath, toluene recycle after separation into solvent recovery slot；
6) carbonaceous mesophase spherules after cleaning enter tray drier drying by charger, 350 DEG C of drying temperature, dry
Time 30min；
7) carbonaceous mesophase spherules after drying enter blade cooler and are cooled to room temperature, and it is micro- to be packaged to be finished product mesocarbon
Ball；The flue gas scripture that the asphalt stock slot, reaction kettle, subsider, sedimentation liquid head tank, centrifuge, tray drier generate
Family name's Guan Houyong washing oil absorbs reuse, and residual gas is through burning disposal.
As shown in figure 4, a kind of system that thermal polycondensation process prepares carbonaceous mesophase spherules in the present embodiment, including asphalt stock slot
1, reaction kettle 2, subsider 3, sedimentation liquid head tank 4, washing oil head tank 5, centrifuge 6, mother liquor tank 7, washing oil slot 8, solvent tank
16, solvent head tank 9, solvent recovery slot 10, driving conveying device 11, charger 12, tray drier 13, paddle cooler
14, packing apparatus 15 and smoke depressant systems, the discharge port of the asphalt stock slot 1 pass through pipeline equipped with pump and reaction kettle 2 into
The discharge port of material mouth connection, reaction kettle 2 is connect by pipeline with the mother liquor bitumen feed mouth of subsider 3, the discharge port of subsider 3
Pipeline by being equipped with oil pump connect with the feed inlet of sedimentation liquid head tank 4, the discharge port of sedimentation liquid head tank 4 pass through pipeline and
The sedimentation liquid feed inlet of centrifuge 6 connects, and the discharge port of washing oil head tank 5 is arranged threeway, a discharge end by pipeline with
The washing oil feed inlet of subsider 3 connects, another discharge end is connect by pipeline with the washing oil feed inlet of centrifuge 6, washing oil
The discharge port of slot 8 is connect by pipeline with the feed inlet of washing oil head tank 5, and the discharge port of solvent tank 16 passes through pipeline and solvent
The feed inlet of head tank 9 connects, and the discharge port of solvent head tank 9 is connect by pipeline with the solvent feed mouth of centrifuge 6, is centrifuged
6 cleaning agent of machine outlet setting threeway, a discharge end are connect by pipeline with the feed inlet of mother liquor tank 7, another discharge end
Mouth is connect by pipeline with the feed inlet of solvent recovery slot 10, and 6 solid phase discharge port of centrifuge is arranged in driving conveying device 11
The underface of driving 11 feed opening of conveying device, the discharge port and disk of charger 12 is arranged in side, the feed inlet of charger 12
The feed inlet of formula drying machine 13 connects, and the discharge port of tray drier 13 is connect with the feed inlet of paddle cooler 14, and paddle is cold
But packing apparatus 15 is arranged in the discharge outlet of machine 14, and the smoke depressant systems successively absorb slot and incineration system by Venturi tube, washing oil
Connection composition, the reaction kettle 2, subsider 3, sedimentation liquid head tank 4, centrifuge 6 and tray drier 11 smoke outlet pass through
The connection of the Venturi tube smoke inlet of pipeline and smoke depressant systems.
Embodiment 2
The method that one of the present embodiment thermal polycondensation process prepares carbonaceous mesophase spherules, includes the following steps:
1) raw material coal tar pitch is put into asphalt stock slot, is warming up to 200 DEG C, and constant temperature to pitch liquefies, and it is former to obtain liquid phase pitch
Material；The coal tar pitch softening point is 75-80 DEG C, quinoline insolubles≤4%.
2) input of liquid phase asphalt stock has the reaction kettle of blender, and inert gas shielding is warming up to 450 DEG C, pressure
0.7MPa, mixing speed 400r/min, constant temperature thermal polycondensation 5h obtain the mother liquor pitch rich in mesophasespherule；
3) washing oil that the subsider with blender is previously implanted, the amount for being previously implanted subsider washing oil is mother liquor pitch body
Mother liquor pitch containing mesophasespherule is inputted subsider from reaction kettle while stirring to after 150 DEG C by long-pending 1/2, constant temperature,
Input speed control settlement bath temperature rise be no more than 10 DEG C/min, mixing speed 400r/min, constant temperature to 150 DEG C, residence time 1h,
Mesophasespherule settles out to form carbonaceous mesophase spherules, obtains the sedimentation liquid containing carbonaceous mesophase spherules；
4) the sedimentation liquid pump containing carbonaceous mesophase spherules is delivered to the sedimentation liquid head tank with blender, mixing speed
400r/min, constant temperature is to 120 DEG C；
5) sedimentation liquid after constant temperature is delivered to centrifuge from sedimentation liquid head tank and carries out high temperature centrifugal filtration separation, is centrifuged
Filtering temperature is 120 DEG C, and the carbonaceous mesophase spherules isolated first carry out cleaning 2 times with toluene in centrifuge；Then washing oil is used again
Cleaning 4 times is carried out, toluene and each dosage of washing oil are 2 times of carbonaceous mesophase spherules quality, clean the toluene of carbonaceous mesophase spherules
Temperature with washing oil is 50 DEG C, centrifuge speed 15000r/min, and the washing oil after the liquid being centrifugated out and cleaning is recycled to
Mother liquor tank, toluene recycle after separation into solvent recovery slot；
6) carbonaceous mesophase spherules after cleaning enter tray drier drying by charger, 420 DEG C of drying temperature, dry
Time 15min；
7) carbonaceous mesophase spherules after drying enter blade cooler and are cooled to room temperature, and it is micro- to be packaged to be finished product mesocarbon
Ball；The flue gas scripture that the asphalt stock slot, reaction kettle, subsider, sedimentation liquid head tank, centrifuge, tray drier generate
Family name's Guan Houyong washing oil absorbs reuse, and residual gas is through burning disposal.
The structure and the phase in embodiment 1 that one of the present embodiment thermal polycondensation process prepares the system of carbonaceous mesophase spherules
Together.
Embodiment 3
The method that one of the present embodiment thermal polycondensation process prepares carbonaceous mesophase spherules, includes the following steps:
1) raw material coal tar pitch is put into asphalt stock slot, is warming up to 180 DEG C, and constant temperature to pitch liquefies, and it is former to obtain liquid phase pitch
Material；The coal tar pitch softening point is 75-80 DEG C, quinoline insolubles≤4%.
2) input of liquid phase asphalt stock has the reaction kettle of blender, and inert gas shielding is warming up to 420 DEG C, pressure
0.6a, mixing speed 300r/min, constant temperature thermal polycondensation 6h obtain the mother liquor pitch rich in mesophasespherule；
3) washing oil that the subsider with blender is previously implanted, the amount for being previously implanted subsider washing oil is mother liquor pitch body
Mother liquor pitch containing mesophasespherule after 130 DEG C, is inputted subsider from reaction kettle while stirring by long-pending 1/3, constant temperature,
Input speed control settlement bath temperature rise be no more than 10 DEG C/min, mixing speed 300r/min, constant temperature to 130 DEG C, residence time 3h,
Mesophasespherule settles out to form carbonaceous mesophase spherules, obtains the sedimentation liquid containing carbonaceous mesophase spherules；
4) the sedimentation liquid pump containing carbonaceous mesophase spherules is delivered to the sedimentation liquid head tank with blender, mixing speed
300r/min, constant temperature is to 110 DEG C；
5) sedimentation liquid after constant temperature is delivered to centrifuge from sedimentation liquid head tank and carries out high temperature centrifugal filtration separation, is centrifuged
Filtering temperature is 110 DEG C, and the carbonaceous mesophase spherules isolated first carry out cleaning 2 times with toluene in centrifuge；Then washing oil is used again
Cleaning 3 times is carried out, toluene and each dosage of washing oil are 2 times of carbonaceous mesophase spherules quality, clean the toluene of carbonaceous mesophase spherules
Temperature with washing oil is 40 DEG C, centrifuge speed 12000r/min, and the washing oil after the liquid being centrifugated out and cleaning is recycled to
Mother liquor tank, toluene recycle after separation into solvent recovery slot；
6) carbonaceous mesophase spherules after cleaning enter tray drier drying by charger, 400 DEG C of drying temperature, dry
Time 20min；
7) carbonaceous mesophase spherules after drying enter blade cooler and are cooled to room temperature, and it is micro- to be packaged to be finished product mesocarbon
Ball；The flue gas scripture that the asphalt stock slot, reaction kettle, subsider, sedimentation liquid head tank, centrifuge, tray drier generate
Family name's Guan Houyong washing oil absorbs reuse, and residual gas is through burning disposal.
The structure and the phase in embodiment 1 that one of the present embodiment thermal polycondensation process prepares the system of carbonaceous mesophase spherules
Together.
Claims (10)
1. a kind of method that thermal polycondensation process prepares carbonaceous mesophase spherules, which comprises the steps of:
1) material asphalt is put into asphalt stock slot, is warming up to 150-200 DEG C, and constant temperature to pitch liquefies, and obtains liquid phase asphalt stock；
2) input of liquid phase asphalt stock has the reaction kettle of blender, and inert gas shielding is warming up to 400-450 DEG C, pressure
0.5-0.7MPa, mixing speed 200-400r/min, constant temperature thermal polycondensation 5-7h obtain the mother liquor rich in mesophasespherule and drip
It is green；
3) washing oil that is previously implanted of subsider with blender, constant temperature will contain interphase to after 100-150 DEG C while stirring
Spherular mother liquor pitch inputs subsider, mixing speed 200-400r/min from reaction kettle, and constant temperature is stopped to 100-150 DEG C
Time 1-5h, mesophasespherule settle out to form carbonaceous mesophase spherules, obtain the sedimentation liquid containing carbonaceous mesophase spherules；
4) the sedimentation liquid pump containing carbonaceous mesophase spherules is delivered to the sedimentation liquid head tank with blender, mixing speed 200-
400r/min, constant temperature is to 100-120 DEG C；
5) sedimentation liquid after constant temperature is delivered to centrifuge centrifuge separation from sedimentation liquid head tank, and the carbonaceous mesophase spherules isolated exist
It is first cleaned with toluene in centrifuge, is then cleaned again with washing oil, centrifuge speed 8000-15000r/min；
6) carbonaceous mesophase spherules after cleaning enter tray drier drying by charger, 350-420 DEG C of drying temperature, dry
Time 15-30min；
7) carbonaceous mesophase spherules after drying enter blade cooler and are cooled to room temperature, and are packaged to be finished product carbonaceous mesophase spherules.
2. the method that a kind of thermal polycondensation process according to claim 1 prepares carbonaceous mesophase spherules, it is characterised in that: the step
It is rapid 1) in material asphalt be coal tar pitch, softening point be 75-80 DEG C, quinoline insolubles≤4%.
3. the method that a kind of thermal polycondensation process according to claim 2 prepares carbonaceous mesophase spherules, it is characterised in that: the step
It is rapid 3) in be previously implanted subsider washing oil amount be mother liquor pitch volume 1/4-1/2.
4. the method that a kind of thermal polycondensation process according to claim 3 prepares carbonaceous mesophase spherules, it is characterised in that: the step
It is rapid 3) in the mother liquor pitch containing mesophasespherule from reaction kettle input subsider speed control subsider temperature rise be no more than
10℃/min。
5. the method that a kind of thermal polycondensation process according to claim 4 prepares carbonaceous mesophase spherules, it is characterised in that: the step
Rapid 5) the middle specific method being centrifugated is high temperature centrifugal filtration, and centrifugal filtration temperature is 100-120 DEG C.
6. the method that a kind of thermal polycondensation process according to claim 5 prepares carbonaceous mesophase spherules, it is characterised in that: the step
It is rapid 5) in the toluene of cleaning carbonaceous mesophase spherules and the temperature of washing oil be 30-50 DEG C, toluene cleans 1-2 times, during each dosage is
Between 1-2 times of phase carbosphere quality, washing oil cleans 2-4 time, and each dosage is 1-2 times of carbonaceous mesophase spherules quality.
7. the method that a kind of thermal polycondensation process according to claim 6 prepares carbonaceous mesophase spherules, it is characterised in that: the step
It is rapid 5) in washing oil after the liquid that is centrifugated out and cleaning be recycled to mother liquor tank, toluene recycles after separation into solvent recovery slot
It utilizes.
8. the method that a kind of thermal polycondensation process according to claim 7 prepares carbonaceous mesophase spherules, it is characterised in that: the drip
The flue gas that green raw material tank, reaction kettle, subsider, sedimentation liquid head tank, centrifuge, tray drier generate is after Venturi tube with washing
Oil absorbs reuse, and residual gas is through burning disposal.
9. the system that a kind of thermal polycondensation process prepares carbonaceous mesophase spherules, it is characterised in that: including asphalt stock slot (1), reaction kettle
(2), subsider (3), sedimentation liquid head tank (4), washing oil head tank (5), centrifuge (6), mother liquor tank (7), washing oil slot (8), molten
Agent storage tank (16), solvent head tank (9), solvent recovery slot (10), driving conveying device (11), charger (12), tray drying
Machine (13), paddle cooler (14) and packing apparatus (15),
The discharge port of the asphalt stock slot (1) passes through the pipeline equipped with pump and connect with the feed inlet of reaction kettle (2), reaction kettle
(2) discharge port is connect by pipeline with the mother liquor bitumen feed mouth of subsider (3), and the discharge port of subsider (3) is by being equipped with
The pipeline of oil pump is connect with the feed inlet of sedimentation liquid head tank (4), and the discharge port of sedimentation liquid head tank (4) passes through pipeline and centrifugation
The sedimentation liquid feed inlet of machine (6) connects, and the discharge port of washing oil head tank (5) is arranged threeway, a discharge end by pipeline with
The washing oil feed inlet of subsider (3) connects, another discharge end is connect by pipeline with the washing oil feed inlet of centrifuge (6),
The discharge port of washing oil slot (8) is connect by pipeline with the feed inlet of washing oil head tank (5), and the discharge port of solvent tank (16) passes through
Pipeline is connect with the feed inlet of solvent head tank (9), and the discharge port of solvent head tank (9) is molten by pipeline and centrifuge (6)
The connection of agent feed inlet, centrifuge (6) cleaning agent outlet setting threeway, discharge end by pipeline and mother liquor tank (7) into
Material mouth connection, another discharge end are connect by pipeline with the feed inlet of solvent recovery slot (10), are driven a vehicle conveying device (11)
It is arranged in the side of centrifuge (6) solid phase discharge port, the feed inlet setting of charger (12) is in driving conveying device (11) blanking
The underface of mouth, the discharge port of charger (12) are connect with the feed inlet of tray drier (13), and tray drier (13) goes out
Material mouth is connect with the feed inlet of paddle cooler (14), and packing apparatus (15) are arranged in the discharge outlet of paddle cooler (14).
10. the system that thermal polycondensation process according to claim 9 prepares carbonaceous mesophase spherules, it is characterised in that: the preparation
The system of carbonaceous mesophase spherules further includes smoke depressant systems, and smoke depressant systems successively absorb slot by Venturi tube, washing oil and incineration system connects
Connect composition, the reaction kettle (2), subsider (3), sedimentation liquid head tank (4), centrifuge (6) and tray drier (11) row
Mouth is connected by the Venturi tube smoke inlet of pipeline and smoke depressant systems.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811051791.5A CN109179367B (en) | 2018-09-10 | 2018-09-10 | Method and system for preparing mesocarbon microbeads by thermal polycondensation method |
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