CN105271168B - The method for continuously preparing carbonaceous mesophase spherules coproduction dipping agent bitumen and cladding pitch - Google Patents
The method for continuously preparing carbonaceous mesophase spherules coproduction dipping agent bitumen and cladding pitch Download PDFInfo
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- CN105271168B CN105271168B CN201510686883.0A CN201510686883A CN105271168B CN 105271168 B CN105271168 B CN 105271168B CN 201510686883 A CN201510686883 A CN 201510686883A CN 105271168 B CN105271168 B CN 105271168B
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Abstract
A kind of method for continuously preparing carbonaceous mesophase spherules coproduction dipping agent bitumen and cladding pitch, is carried out according to the following steps：（1）Under the conditions of nitrogen atmosphere, medium temperature coal pitch is mixed with stabilizer；（2）Quick temperature raising device is sent into after being heated to 350 ~ 380 DEG C, and being warming up to 410 ~ 450 DEG C in the time of 1 ~ 5s carries out polymerisation；（3）290 ~ 340 DEG C are cooled to extractant hybrid extraction；（4）Centrifugation, solid phase are dried and obtain carbonaceous mesophase spherules product；（5）Mother liquor reclaims extractant using destilling tower evaporation, and the remaining material of bottom of towe carries out modification reaction as dipping agent bitumen or using modification reactor.The problems such as method of the present invention fundamentally solves big traditional processing technology energy resource consumption, environmental pollution weight, low product yield, high cost, unstable quality and single varieties.
Description
Technical field
The present invention relates to carbonaceous mesophase spherules field of material technology, more particularly to one kind continuously prepare carbonaceous mesophase spherules connection
The method for producing dipping agent bitumen and cladding pitch.
Background technology
Negative material is one of the key factor for affecting performance of lithium ion battery, general in prior art using graphite or changes
Property graphite, but its theoretical embedding lithium capacity 372mAh/g can not meet demand, at the same its distinctive layer structure cause limited
Secondary cyclical stability, and also extremely sensitive to electrolyte, therefore urgently need to look for a kind of negative pole material of new replacement graphite
Material.
Carbonaceous mesophase spherules are the negative material raw materials of more satisfactory lithium ion battery.At present, with coal tar asphalt it is
Raw material produces the technique of carbonaceous mesophase spherules, mainly has thermal polycondensation process, emulsion process and suspension method, adopts in industrialized production
Batch production technique.
Thermal polycondensation process batch production technique be first material in polymeric kettle is carried out persistently overheating, after reaching set point of temperature
Insulation operation is carried out, whole cycle needs 16 ~ 20 hours.The production technology is low due to the warming-up device thermal efficiency, energy utilization rate
Not high so that energy resource consumption is higher, pollutant discharge amount increases.And there are problems that product is single, production cost, meanwhile,
In polymeric kettle coal tar asphalt contact with polymeric kettle inwall partially due to long-time overheated, cause coal tar asphalt in polymeric kettle
Inwall coking phenomenon is serious, reduces the heat transfer efficiency of polymeric kettle, causes the production cycle in production process to extend, and energy resource consumption increases
Plus, unstable product quality.
Emulsion process is easily brought impurity in product into due to introducing dispersant in process of production, meanwhile, using emulsification
The carbonaceous mesophase spherules of method production have fusible property, need to do oxidation-stabilized process, technical process in subsequent technique
Complexity, production cost height, low raw material availability, unstable product quality and product category is single.
Suspension method needs multiple organic solvents and suspension in process of production, through high temperature balling-up, cooling, filter analysis, pre-
The multiple operation such as oxidation, carbonization makes carbonaceous mesophase spherules, also there is complex technical process, production cost height, raw material and utilizes
Rate is low, the problem that unstable product quality and product category are single.
《Aerospace material technique》The 6th periodical of calendar year 2001 is sent out《The preparation and its embedding lithium behavior of mesophase pitch carbosphere
Research》A kind of method of typical thermal polymerization legal system carbonaceous mesophase spherules is described, 250 are warmed up to first under nitrogen protection
DEG C, heating stirring 1h removes the small molecule for being difficult to be polymerized, and is then being warmed up to 450 DEG C from liter pressure, polymerisation 2h；Reaction
Product heat filtering at 150 DEG C, to colourless or faint yellow, finally at 80 DEG C, vacuum drying 6h is filtration product pyridine extraction
Obtain MCMB（Carbonaceous mesophase spherules）；The method increased the operation difficulty in production process by the way of two sections of polymerizations；Dividing
During difficult polymerization small molecule, inevitably cause the loss of raw material to increase, reduce raw material availability and product
Yield；Meanwhile, the technique equally has common fault present in thermal polymerization batch production process.
Content of the invention
For existing carbonaceous mesophase spherules in the problems referred to above present on technology of preparing, the present invention provides a kind of continuous preparation
Carbonaceous mesophase spherules coproduction dipping agent bitumen and the method for cladding pitch, are connected using thermal polymerization by continuous Preparation equipment
Continuous production, solves the problems such as energy resource consumption is big, environmental pollution is heavy, obtains stay-in-grade multiple product.
The method of the present invention is carried out according to the following steps：
1st, under the conditions of nitrogen atmosphere, it is 180 ~ 210 DEG C steady by temperature for 180 ~ 210 DEG C of medium temperature coal pitch and temperature
Determine agent mixing, mixed proportion is medium temperature coal pitch in mass ratio:Stabilizer=1:（0.1～1）, obtain mixed material；Described is steady
Agent is determined for steam, washing oil or carbolineum；
2nd, quick temperature raising device is sent into after mixed material being heated to 350 ~ 380 DEG C, and material is in 1 ~ 5s in the quick temperature raising device
Time be warming up to 410 ~ 450 DEG C, carry out polymerisation subsequently into continuous polymerization reactor at 410 ~ 450 DEG C, control middle temperature
The material that reaction time of the coal tar pitch in continuous polymerization reactor is discharged from continuous polymerization reactor after the completion of 4 ~ 6h, reaction
Polymerbitumen containing carbonaceous mesophase spherules；
3rd, the polymerbitumen containing carbonaceous mesophase spherules is cooled to 290 ~ 340 DEG C, then after mixing with extractant, sends into extraction
Take groove to be extracted, mixed proportion is the polymerbitumen containing carbonaceous mesophase spherules according to mass ratio:Extractant=1:（1~5）；
Control extraction temperature is extracted 2 ~ 5 hours at 120 ~ 180 DEG C, and material after then being extracted, wherein containing carbonaceous mesophase spherules
During unreacted material in polymerbitumen is by solvent extraction to extractant；Described extractant is washing oil or carbolineum；
4th, material after extraction is separated by filtration with centrifuge, isolates solid phase and mother liquor, control solid portion in solid phase
Diameter >=2 μm, solid phase are dried and remove liquid portion, obtain carbonaceous mesophase spherules product；
Mother liquor is reclaimed extraction using destilling tower evaporation by the 5th, 2 μm of the diameter ＜ of the solid portion contained in the mother liquor for obtaining
Agent, the remaining material of bottom of towe carry out modification reaction as dipping agent bitumen or using modification reactor, or simultaneously as leaching
Stain agent pitch and using modification reactor carry out modification reaction；Material after the completion of modification reaction enters the abjection volatilization of devolatilization machine
Point, obtain cladding pitch.
In said method, modification reaction is to be passed through, into modification reactor, the hot-air that temperature is at 140 ~ 200 DEG C, keeps kettle
Interior temperature is reacted at 240 ~ 300 DEG C, and the reaction time is 4 ~ 8h.
In said method, equipment that step 2 is adopted for for producing the continuous polymerization reactor of MCMB, including
Housing and it is arranged on the quick temperature raising device of case top, double stirring transmission devices；Case top is provided with nitrogen mouth, and bottom is provided with puts
Material mouth, outside setting chuck, enclosure interior are provided with gate stirrer and shunting main agitator with described double stirrings transmission dresses
Put and be assembled together；Described quick temperature raising device is tubular heat exchanger, and bottom is provided with material inlet and material outlet, and material goes out
Mouth is connected with enclosure interior；It is fixed with scraper plate group to contact with inner walls on the outside of described gate stirrer, inner side is fixed with
Multiple-layer horizontal baffle plate；The blade group of the shunting main agitator inside gate stirrer is located between adjacent two layers horizontal baffle,
Every layer of horizontal baffle is located between adjacent two layers blade.
In the above-mentioned continuous polymerization reactor for producing MCMB, double stirring transmission devices with its above
Reductor and motor are assembled together.
In the above-mentioned continuous polymerization reactor for producing MCMB, gate stirrer has A frames, B frames and C frames
Three frames, the horizontal sextant angle between each frame are 120, and every layer of blade group of shunting main agitator has four blades, each blade it
Between horizontal sextant angle be 90.
In the above-mentioned continuous polymerization reactor for producing MCMB, the oar of the shunting main agitator first half
Leaf is oblique blade, and its width and horizontal plane have 25 ° of angles, and the blade of lower half is flat paddle leaf, is horizontally disposed with, each blade
Length for housing inner diameter 1/4.
In the above-mentioned continuous polymerization reactor for producing MCMB, gate stirrer bottom is provided with sleeve,
Sleeve is connected by sliding bearing with outer stirring support base, and outer stirring support base is fixed on outer casing inner wall by outer stirring bracing frame
On；Shunting main agitator bottom is connected by sliding bearing through sleeve with interior stirring support base, and interior stirring support base passes through
Interior stirring bracing frame is fixed on outer casing inner wall.
The length of above-mentioned horizontal baffle for housing inner diameter 1/3.
The tubulation external diameter of above-mentioned tubular heat exchanger is 19mm, and tubulation quantity is 30 ~ 80.
In the above-mentioned continuous polymerization reactor for producing MCMB, fix on each frame of gate stirrer
Scraper plate group is made up of the multiple scraper plates for being located at same facade, and each scraper plate specification is 150mm × 50mm, longitudinally mounted, on each frame
Adjacent from top to bottom two scraper plate spacing be 240mm；The scraper plate of fixed highest point and A arch position wherein on A frames
Top 130mm of the scraper plate of fixed highest point less than B frames on sustained height, B frames, the scraper plate of fixed highest point on C frames
Top 260mm less than B frames.
In the above-mentioned continuous polymerization reactor for producing MCMB, the top of housing is elliptic end socket,
Middle part is core structure, and bottom is pyramidal structure.
In said method, recovered solvent is reused.
The above-mentioned using method for producing the continuous polymerization reactor of MCMB is：
1st, nitrogen is passed through to enclosure interior by nitrogen mouth, by the air row in housing and inside the tubulation of quick temperature raising device
Go out；Then nitrogen mouth is closed；
The 2nd, the material to be polymerized that temperature is 350 ~ 380 DEG C is passed through the material inlet of quick temperature raising device, from quick temperature raising device
Bottom enters tubulation, with the fused salt heat exchanging entered in quick temperature raising device, within the time of 1 ~ 5 second is preheated to material to be polymerized
420 ~ 460 DEG C, then enter in housing from material outlet；Described material to be polymerized is medium temperature coal pitch；
3rd, double stirring transmission devices are opened, gate stirrer and shunting main agitator counter-rotating, rotary speed point is made
Not Wei shunting 50 ~ 70r/min of main agitator, gate stirrer 10r/min makes material to be polymerized carry out polymerisation；While to
It is passed through fused-salt medium to be incubated in chuck, or is incubated using infrared electric heating；
4th, after stable reaction, by the continuous blowing of drain hole, and material inlet continuous feed, new in polymerization process
Interface between the MCMB and mid temperature pitch of generation is constantly updated, the MCMB generated after fully reacting
It is discharged.
Described material to be polymerized is medium temperature coal pitchWithThe mixed material of stabilizer.
The method of the present invention adopts continuous feeding device, by design material proportion, through continuous polymerization, solvent extraction, from
The heart is separated and the steps such as solvent recovery, fundamentally solves big traditional processing technology energy resource consumption, environmental pollution weight, product receipts
Rate is low, high cost, unstable quality and the problems such as single varieties；Using continuous polymerization reactor fused salt can be made to carry out with pitch
Indirect heat exchange, pitch firing rate are fast, it is to avoid asphalt coking；By gate stirrer and the main stirring of shunting of counter-rotating
Device, makes blade shear material with horizontal baffle, and partial material is moved to housing upper, and reactive polymeric effect is with anti-
Prolongation between seasonable and more uniform, make the uniform fast growth of MCMB, the paddle belt of wherein top is angled, can
Fully ensure that the material on top is moved upwards, reach optimal reflowing result；Scraper plate is by the material scraping of housing sidewall, it is to avoid material
Wall built-up, coking；Pitch is while reactor top is constantly moved upwards, and is cut by three gate stirrers of different directions
Cut, the interface in polymerization process between newly-generated MCMB and pitch is constantly updated, in further promoting
Between the uniform fast growth of phase carbon microspheres.
Description of the drawings
The sides that continuously prepare carbonaceous mesophase spherules coproduction dipping agent bitumen and cladding pitch of the Fig. 1 for the embodiment of the present invention 1
Method schematic flow sheet；
Fig. 2 is the continuous polymerization reactor structural representation for producing MCMB in the embodiment of the present invention；
Fig. 3 is scraped for each frame that the structure in the embodiment of the present invention is used for the continuous polymerization reactor for producing MCMB
Plate structure schematic diagram；Wherein（a）For the scraper plate of A frames,（b）For the scraper plate of B frames,（c）Scraper plate for C frames；
F-F face sectional views of the Fig. 4 for Fig. 2；
D-D face sectional views of the Fig. 5 for Fig. 2；
In figure, 1, quick temperature raising device, 2, housing, 3, chuck, 4, interior stirring bracing frame, 5, outer stirring bracing frame, 6, flat paddle
Leaf, 7, oblique blade, 8, gate stirrer, 9, mechanical seal cooling jacket, 10, interior stirring sealing, 11, outer stirring sealing, 12, double
Stirring transmission device, 13, reductor, 14, motor, 15, scraper plate, 16, horizontal baffle, 17, shunting main agitator, 18, row
Pipe, 19, quick temperature raising device shell, a, chuck import, b, drain hole, c, JO, d, nitrogen mouth, e, cooling water inlet, f,
Coolant outlet, g, material outlet, h, material inlet, i, quick temperature raising device shell Heating medium, j, quick temperature raising device shell heat
Matchmaker exports, A, A frame, B, B frame, C, C frame.
Specific embodiment
The double stirring transmission devices adopted in the embodiment of the present invention are for gear reduction unit.
It is used for producing the continuous polymerization reactor structure of MCMB in the embodiment of the present invention as shown in Fig. 1,3 and 4,
Including housing 2 and be arranged on case top quick temperature raising device 1, double stirring transmission device 12；Nitrogen mouth d is provided with the top of housing 2,
Bottom is provided with drain hole b, outside chuck 3 is set, be provided with inside housing 2 gate stirrer 8 and shunting main agitator with described
Double stirring transmission devices 12 be assembled together；Described quick temperature raising device 1 is tubular heat exchanger, and bottom is provided with material inlet
H and material outlet g, material outlet g are connected with inside housing 1；The outside of described gate stirrer 8 is fixed with scraper plate group and shell
2 inwall of body is contacted, and inner side is fixed with multiple-layer horizontal baffle plate 16；The blade group of the shunting main agitator inside gate stirrer 8
It is located between adjacent two layers horizontal baffle 16, every layer of horizontal baffle 16 is located between adjacent two layers blade；
Double stirring transmission devices 12 with its above reductor 13 and motor 14 be assembled together；
Gate stirrer 8 has A frames, three frames of B frames and C frames, and the horizontal sextant angle between each frame is 120, the main stirring of shunting
Every layer of blade group of device has four blades, and the horizontal sextant angle between each blade is 90；
The blade of the shunting main agitator first half is oblique blade 7, and its width and horizontal plane have 25 ° of angles, lower half
The blade in portion is flat paddle leaf 6, is horizontally disposed with, and the length of each blade is the 1/4 of 2 internal diameter of housing；
8 bottom of gate stirrer is provided with sleeve, and sleeve is connected by sliding bearing with outer stirring support base, and outer stirring is supported
Seat is fixed on 2 inwall of shell by outer stirring bracing frame 5；Shunting main agitator bottom is through sleeve and interior stirring support base
Connected by sliding bearing, interior stirring support base is fixed on 2 inwall of shell by interior stirring bracing frame 4；
The length of horizontal baffle 16 for 2 internal diameter of housing 1/3；
The tubulation external diameter of tubular heat exchanger is 19mm, and tubulation quantity is 50；
On each frame of gate stirrer 8, fixed scraper plate group is made up of the multiple scraper plates 15 for being located at same facade, and structure is such as
Shown in Fig. 2, each scraper plate specification is 150mm × 50mm, longitudinally mounted, adjacent from top to bottom two scraper plate 15 on each frame
Spacing is 240mm；Wherein on A frames, the scraper plate 15 of fixed highest point is located at sustained height with A arch, fixes most on B frames
Top 130mm of the scraper plate 15 of eminence less than B frames, top 260mm of the scraper plate 15 of fixed highest point less than B frames on C frames；
The top of housing 2 is elliptic end socket, and middle part is core structure, and bottom is pyramidal structure；
The using method of continuous polymerization reactor for being used for producing MCMB in the embodiment of the present invention is：
1st, nitrogen is passed through to enclosure interior by nitrogen mouth, by the air row in housing and inside the tubulation of quick temperature raising device
Go out；Then nitrogen mouth is closed；
The 2nd, the material to be polymerized that temperature is 350 ~ 380 DEG C is passed through the material inlet of quick temperature raising device, from quick temperature raising device
Bottom enters tubulation, with the fused salt heat exchanging entered in quick temperature raising device, within the time of 1 ~ 5 second is preheated to material to be polymerized
420 ~ 460 DEG C, then enter in housing from material outlet；Described material to be polymerized is medium temperature coal pitch；
3rd, double stirring transmission devices are opened, gate stirrer and shunting main agitator counter-rotating, rotary speed point is made
Not Wei shunting 50 ~ 70r/min of main agitator, gate stirrer 10r/min makes material to be polymerized carry out polymerisation；While to
It is passed through fused-salt medium to be incubated in chuck, or is incubated using infrared electric heating；
4th, after stable reaction, by the continuous blowing of drain hole, and material inlet continuous feed, new in polymerization process
Interface between the MCMB and mid temperature pitch of generation is constantly updated, the MCMB generated after fully reacting
It is discharged.
In the embodiment of the present invention, the yield of carbonaceous mesophase spherules is more than 25%, the quality index of carbonaceous mesophase spherules product
For fixed carbon >=95%, real density 0.75g/cm3, volatile matter 8 ~ 12%, moisture≤0.3%.
In the embodiment of the present invention when adopting stabilizer for steam, moisture is isolated with oil water separator during recycling design
Go.
When carrying out modification reaction in the embodiment of the present invention, the flow of hot-air is 1 ~ 1.5m3/h.
Embodiment 1
Under the conditions of nitrogen atmosphere, the medium temperature coal pitch that temperature is 180 DEG C is mixed with the stabilizer that temperature is 180 DEG C,
Mixed proportion is medium temperature coal pitch in mass ratio:Stabilizer=1:0.1, obtain mixed material；Described stabilizer is carbolineum；
Quick temperature raising device is sent into after mixed material is heated to 350 DEG C, time liter of the material in 1s in the quick temperature raising device
Temperature carries out polymerisation subsequently into continuous polymerization reactor at 410 DEG C to 410 DEG C, and control medium temperature coal pitch is in continuous polymerization
The material that reaction time in reactor is discharged from continuous polymerization reactor after the completion of 6h, reaction contains carbonaceous mesophase spherules
Polymerbitumen；
Polymerbitumen containing carbonaceous mesophase spherules is cooled to 290 DEG C, then after mixing with extractant, sends into extraction tank
Row extraction, mixed proportion is the polymerbitumen containing carbonaceous mesophase spherules according to mass ratio:Extractant=1:5；Control extraction temperature
Degree is extracted 5 hours at 120 DEG C, not anti-in material after then being extracted, the wherein polymerbitumen containing carbonaceous mesophase spherules
During material is answered by solvent extraction to extractant；Described extractant is carbolineum；
Material after extraction is separated by filtration with centrifuge, solid phase and mother liquor is isolated, solid portion is straight in control solid phase
Footpath >=2 μm, solid phase are dried and remove liquid portion, obtain carbonaceous mesophase spherules product；
Mother liquor is reclaimed extractant using destilling tower evaporation by 2 μm of the diameter ＜ of the solid portion contained in the mother liquor of acquisition,
The remaining material of bottom of towe is used as dipping agent bitumen；
In said method, equipment that step 2 is adopted is for for producing the continuous polymerization reactor of MCMB；
In said method, recovered solvent is reused.
Embodiment 2
With embodiment 1, difference is method：
（1）Under the conditions of nitrogen atmosphere, the medium temperature coal pitch that temperature is 210 DEG C and the stabilizer that temperature is 210 DEG C are mixed
Close, mixed proportion is medium temperature coal pitch in mass ratio:Stabilizer=1:0.5, obtain mixed material；Described stabilizer is washing oil；
（2）Quick temperature raising device is sent into after mixed material is heated to 360 DEG C, time of the material in 3s in the quick temperature raising device
430 DEG C being warming up to, polymerisation being carried out subsequently into continuous polymerization reactor at 430 DEG C, control medium temperature coal pitch is continuously gathering
The reaction time in reactor is closed in 5h；
（3）Polymerbitumen containing carbonaceous mesophase spherules is cooled to 310 DEG C, then after mixing with extractant, sends into extraction tank
Extracted, mixed proportion is the polymerbitumen containing carbonaceous mesophase spherules according to mass ratio:Extractant=1:3；Control extraction
Temperature is extracted 4 hours at 150 DEG C；Described extractant is washing oil；
（4）The remaining material of bottom of towe carries out modification reaction using modification reactor, and the material after the completion of modification reaction is entered
Volatile matter deviate from by devolatilization machine, obtains cladding pitch；Wherein modification reaction is into modification reactor to be passed through temperature at 140 ~ 200 DEG C
Hot-air, keep temperature in the kettle reacted at 240 ~ 300 DEG C, the reaction time is 8h.
Embodiment 3
With embodiment 1, difference is method：
（1）Under the conditions of nitrogen atmosphere, the medium temperature coal pitch that temperature is 200 DEG C and the stabilizer that temperature is 20 DEG C are mixed
Close, mixed proportion is medium temperature coal pitch in mass ratio:Stabilizer=1:1, obtain mixed material；Described stabilizer is steam；
（2）Quick temperature raising device is sent into after mixed material is heated to 380 DEG C, time of the material in 5s in the quick temperature raising device
450 DEG C being warming up to, polymerisation being carried out subsequently into continuous polymerization reactor at 450 DEG C, control medium temperature coal pitch is continuously gathering
The reaction time in reactor is closed in 4h；
（3）Polymerbitumen containing carbonaceous mesophase spherules is cooled to 340 DEG C, then after mixing with extractant, sends into extraction tank
Extracted, mixed proportion is the polymerbitumen containing carbonaceous mesophase spherules according to mass ratio:Extractant=1:1；Control extraction
Temperature is extracted 2 hours at 180 DEG C；Described extractant is washing oil；
（4）Bottom of towe remaining material such as is divided at the two parts of quality, respectively as dipping agent bitumen and using modification reaction
Kettle carries out modification reaction；Material after the completion of modification reaction enters devolatilization machine abjection volatile matter, obtains cladding pitch；Wherein modify
Reaction is to be passed through, into modification reactor, the hot-air that temperature is at 140 ~ 200 DEG C, keeps temperature in the kettle to carry out at 240 ~ 300 DEG C anti-
Should, the reaction time is 4h.
Claims (8)
1. a kind of continuously prepare carbonaceous mesophase spherules coproduction dipping agent bitumen and cladding pitch method, it is characterised in that by following
Step is carried out：
(1) under the conditions of nitrogen atmosphere, it is 180～210 DEG C steady by medium temperature coal pitch and temperature that temperature is 180～210 DEG C
Determine agent mixing, mixed proportion is medium temperature coal pitch in mass ratio:Stabilizer=1:(0.1～1), obtains mixed material；Described
Stabilizer is steam, washing oil or carbolineum；
(2) quick temperature raising device is sent into after mixed material being heated to 350～380 DEG C, and material is 1～5s's in the quick temperature raising device
Time is warming up to 410～450 DEG C, subsequently into carrying out polymerisation at 410～450 DEG C in the housing of continuous polymerization reactor,
Control reaction time of the medium temperature coal pitch in the housing of continuous polymerization reactor is after the completion of 4～6h, reaction from continuous polymerization
The material that reactor is discharged contains the polymerbitumen of carbonaceous mesophase spherules；The equipment for adopting is for for producing MCMB
Continuous polymerization reactor, including housing and is arranged on the quick temperature raising device of case top, double stirring transmission devices；Case top sets
Have a nitrogen mouth, bottom is provided with drain hole, outside chuck is set, enclosure interior be provided with gate stirrer and shunting main agitator with
Described double stirring transmission devices are assembled together；Described quick temperature raising device is tubular heat exchanger, and bottom is provided with material and enters
Mouth and material outlet, material outlet are connected with enclosure interior；Scraper plate group and housing is fixed with the outside of described gate stirrer
Inwall is contacted, and inner side is fixed with multiple-layer horizontal baffle plate；The blade group of the shunting main agitator inside gate stirrer is located at phase
Between adjacent two-layer horizontal baffle, every layer of horizontal baffle is located between adjacent two layers blade；
(3) polymerbitumen containing carbonaceous mesophase spherules is cooled to 290～340 DEG C, then after mixing with extractant, sends into extraction
Groove is extracted, and mixed proportion is the polymerbitumen containing carbonaceous mesophase spherules according to mass ratio:Extractant=1:(1～5)；Control
Extraction temperature processed is extracted 2～5 hours at 120～180 DEG C, and material after then being extracted, wherein containing carbonaceous mesophase spherules
During unreacted material in polymerbitumen is by solvent extraction to extractant；Described extractant is washing oil or carbolineum；
(4) material after extraction is separated by filtration with centrifuge, isolates solid phase and mother liquor, control the diameter of solid portion in solid phase
>=2 μm, solid phase is dried and removes liquid portion, obtain carbonaceous mesophase spherules product；
(5) mother liquor is reclaimed extractant using destilling tower evaporation by 2 μm of the diameter ＜ of the solid portion contained in the mother liquor for obtaining,
The remaining material of bottom of towe carries out modification reaction as dipping agent bitumen or using modification reactor, or simultaneously as impregnating agent
Pitch and using modification reactor carry out modification reaction；Material after the completion of modification reaction enters devolatilization machine abjection volatile matter, obtains
Pitch must be coated.
2. according to claim 1 a kind of continuously prepare carbonaceous mesophase spherules coproduction dipping agent bitumen and cladding pitch side
Method, it is characterised in that in the described continuous polymerization reactor for producing MCMB, double stirring transmission devices and its
The reductor and motor of top is assembled together.
3. according to claim 1 a kind of continuously prepare carbonaceous mesophase spherules coproduction dipping agent bitumen and cladding pitch side
Method, it is characterised in that in the described continuous polymerization reactor for producing MCMB, gate stirrer has A frames, B frames
With three frames of C frames, the horizontal sextant angle between each frame is 120 °, and every layer of blade group of shunting main agitator has four blades, respectively
Horizontal sextant angle between blade is 90 °.
4. according to claim 1 a kind of continuously prepare carbonaceous mesophase spherules coproduction dipping agent bitumen and cladding pitch side
Method, it is characterised in that in the described continuous polymerization reactor for producing MCMB, shunting main agitator upper half
The blade in portion is oblique blade, and its width and horizontal plane have 25 ° of angles, and the blade of lower half is flat paddle leaf, is horizontally disposed with, respectively
The length of blade for housing inner diameter 1/4.
5. according to claim 1 a kind of continuously prepare carbonaceous mesophase spherules coproduction dipping agent bitumen and cladding pitch side
Method, it is characterised in that in the described continuous polymerization reactor for producing MCMB, gate stirrer bottom is provided with
Sleeve, sleeve are connected by sliding bearing with outer stirring support base, and outer stirring support base is fixed outside by outer stirring bracing frame
On shell inwall；Shunting main agitator bottom is connected by sliding bearing through sleeve with interior stirring support base, and interior stirring is supported
Seat is fixed on outer casing inner wall by interior stirring bracing frame.
6. according to claim 1 a kind of continuously prepare carbonaceous mesophase spherules coproduction dipping agent bitumen and cladding pitch side
Method, it is characterised in that in the described continuous polymerization reactor for producing MCMB, on each frame of gate stirrer
Fixed scraper plate group is made up of the multiple scraper plates for being located at same facade, and each scraper plate specification is 150mm × 50mm, longitudinally mounted, per
The spacing of adjacent from top to bottom two scraper plate on individual frame is 240mm；The scraper plate of fixed highest point and A frames wherein on A frames
Top is located at sustained height, top 130mm of the scraper plate of fixed highest point less than B frames on B frames, fixed highest point on C frames
Scraper plate less than B frames top 260mm.
7. according to claim 1 a kind of continuously prepare carbonaceous mesophase spherules coproduction dipping agent bitumen and cladding pitch side
Method, it is characterised in that in the described continuous polymerization reactor for producing MCMB, the top of housing is elliptic
End socket, middle part are core structure, and bottom is pyramidal structure.
8. according to claim 1 a kind of continuously prepare carbonaceous mesophase spherules coproduction dipping agent bitumen and cladding pitch side
Method, it is characterised in that described modification reaction is to be passed through, into modification reactor, the hot-air that temperature is at 140～200 DEG C, keeps
Temperature in the kettle is reacted at 240～300 DEG C, and the reaction time is 4～8h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510686883.0A CN105271168B (en) | 2015-10-22 | 2015-10-22 | The method for continuously preparing carbonaceous mesophase spherules coproduction dipping agent bitumen and cladding pitch |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510686883.0A CN105271168B (en) | 2015-10-22 | 2015-10-22 | The method for continuously preparing carbonaceous mesophase spherules coproduction dipping agent bitumen and cladding pitch |
Publications (2)
| Publication Number | Publication Date |
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| CN105271168A CN105271168A (en) | 2016-01-27 |
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| CN106477549B (en) * | 2016-09-23 | 2019-04-12 | 神华集团有限责任公司 | The separation system and separation method of mesocarbon microspheres |
| CN108075110A (en) * | 2016-11-14 | 2018-05-25 | 微宏动力系统（湖州）有限公司 | Negative electrode for lithium ion battery composite material and lithium ion battery |
| CN106753495A (en) * | 2016-12-29 | 2017-05-31 | 中石化南京工程有限公司 | A kind of method of high temperature coal-tar/residual oil production carbosphere and dipping agent bitumen |
| CN108249417A (en) * | 2017-12-15 | 2018-07-06 | 王强 | A kind of medium temperature coal pitch prepares the device and method of mesocarbon microspheres |
| CN109179367B (en) * | 2018-09-10 | 2020-08-14 | 山西金源煤化科技有限公司 | Method and system for preparing mesocarbon microbeads by thermal polycondensation method |
| CN109868146A (en) * | 2019-03-14 | 2019-06-11 | 山西昭旭科技有限公司 | A kind of medium temperature coal pitch environmental protection and efficiently utilize combined producing process method |
| CN110437863A (en) * | 2019-08-19 | 2019-11-12 | 西安华江环保科技股份有限公司 | A kind of mesocarbon microspheres extraction filter device and method |
| CN113088313B (en) * | 2019-12-23 | 2022-08-12 | 中国石油化工股份有限公司 | Preparation method of mesophase pitch |
| CN112573504B (en) * | 2020-12-31 | 2023-09-15 | 中冶焦耐(大连)工程技术有限公司 | Continuous production process of mesophase carbon microsphere |
| CN113046110B (en) * | 2021-03-19 | 2021-11-23 | 北京旭阳科技有限公司 | Preparation method of binder asphalt, binder asphalt and electrode for aluminum smelting |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1800241A (en) * | 2005-11-30 | 2006-07-12 | 冷亮 | Mesophase asphalt charcoal microsphere preparation method |
| CN201664609U (en) * | 2010-04-15 | 2010-12-08 | 东莞市汇美淀粉科技有限公司 | Mixing reaction pot |
| CN203183993U (en) * | 2013-02-20 | 2013-09-11 | 安徽天意环保科技有限公司 | Preheating device of epoxy reaction kettle |
| CN103833007A (en) * | 2014-03-12 | 2014-06-04 | 中钢集团鞍山热能研究院有限公司 | Preparation method of coal pitch-based mesocarbon microbeads |
| CN104650938A (en) * | 2015-01-12 | 2015-05-27 | 中钢集团鞍山热能研究院有限公司 | Co-production technique of needle coke, mesocarbon microbeads and high-quality asphalt |
-
2015
- 2015-10-22 CN CN201510686883.0A patent/CN105271168B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1800241A (en) * | 2005-11-30 | 2006-07-12 | 冷亮 | Mesophase asphalt charcoal microsphere preparation method |
| CN201664609U (en) * | 2010-04-15 | 2010-12-08 | 东莞市汇美淀粉科技有限公司 | Mixing reaction pot |
| CN203183993U (en) * | 2013-02-20 | 2013-09-11 | 安徽天意环保科技有限公司 | Preheating device of epoxy reaction kettle |
| CN103833007A (en) * | 2014-03-12 | 2014-06-04 | 中钢集团鞍山热能研究院有限公司 | Preparation method of coal pitch-based mesocarbon microbeads |
| CN104650938A (en) * | 2015-01-12 | 2015-05-27 | 中钢集团鞍山热能研究院有限公司 | Co-production technique of needle coke, mesocarbon microbeads and high-quality asphalt |
Non-Patent Citations (2)
| Title |
|---|
| 中间相炭微球的制备与性能;李春艳等;《长沙理工大学学报（自然科学版）》;20130630;第10卷(第2期);第89-92页 * |
| 炭微球制备技术的研究动态;王文志等;《材料导报》;20040731;第18卷(第7期);第62-64页 * |
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Application publication date: 20160127 Assignee: Liaoning Xingde Chemical Co.,Ltd. Assignor: ANSHAN XINGDE MATERIAL SCIENCE & TECHNOLOGY Co.,Ltd. Contract record no.: X2023210000004 Denomination of invention: Method for continuous preparation of mesophase carbon microsphere and co-production of impregnant pitch and coated pitch Granted publication date: 20170315 License type: Exclusive License Record date: 20230202 |