CN109401776A - A kind of method and device of asphalt high-temperature extraction heat - Google Patents
A kind of method and device of asphalt high-temperature extraction heat Download PDFInfo
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- CN109401776A CN109401776A CN201811159942.9A CN201811159942A CN109401776A CN 109401776 A CN109401776 A CN 109401776A CN 201811159942 A CN201811159942 A CN 201811159942A CN 109401776 A CN109401776 A CN 109401776A
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- autoclave
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C3/00—Working-up pitch, asphalt, bitumen
- C10C3/08—Working-up pitch, asphalt, bitumen by selective extraction
Abstract
The invention discloses a kind of method and devices of asphalt high-temperature extraction heat.This method comprises: the preparation of sample;Preparation before extracting;Sample to be extracted is extracted in conjunction with solvent after being crushed, and is collected extract, is closed all heating systems.Extraction equipment includes reactor, condenser pipe, solvent collecting tank and controller, and reactor is by the first autoclave, the second autoclave and the second autoclave composition.The present invention primary property can complete the removing of quinoline insolubles and the recycling of solvent in pitch in one set of instrument, easier compared with existing thermosol technology, fast, environmental protection.The method and device, also can be widely used to other field, such as the extraction and separation of other liquid solvents and solid matter.
Description
Technical field
The invention belongs to a kind of method and devices of asphalt high-temperature extraction heat.
Technical background
Asphalt-based carbon fiber is new high-tech product, is the indispensable material of the sophisticated technologies such as space flight, aviation and military project,
It is the basic raw material of the certain successive generations of products of civilian industry.For a long time, Japan, the U.S. and Germany can produce for manufacturing
General purpose grade asphalt-based carbon fiber spins pitch.Western developed country takes always block policy to China's carbon fiber manufacturing technology,
Only shifted recently as carbon fiber to civilian industry, international community to the manufacturing technology of carbon fiber and products export just
It loosens, and it is still necessary to the special anthorizations of government, exported country for the outlet of general grade carbon fiber complete set technology.
A main bottleneck for restricting universal pitch-based carbon fiber development is exactly that raw material can spin pitch.Asphalt-based carbon fiber
The raw material of production is mainly asphalt, coal tar pitch and naphthalene oligomerisation gained pitch.The former two is by changing to existing pitch
Property and upgrading, the latter are then to regulate and control from source to pitch, but there are complex technical process, catalyst from product pitch
The problems such as separation difficulty, equipment seriously corroded.Main problem existing for road asphalt base carbon fibre has: performance is low, fluctuation is big, even
Continuous spin problems without solution very well, single variety, specification is few, line density is uneven, the lot stability of asphalt stock is very poor.
To find out its cause, the spinnability of mainly pitch does not reach a standard, the various factors of pitch actually can be spun not from theory to influence
On carry out understanding and its structure be not carried out controllably, the quality problems of precursor have become restrict China development asphalt base carbon fiber work
" bottleneck " of industry.
Asphaltene is mainly made of C and H element, separate sources in main preservation and coal tar asphalt and asphalt
Asphaltene be made of polycyclic condensed aromatic hydrocarbon and its alkyl substituents, average molecular weight with higher and armaticity contain
Carbon amounts is high and polymerization or crosslinking easily occurs, and is the presoma for preparing functional Carbon Materials.It realizes stable spinning and produces high property
The primary premise of energy asphalt base carbon fiber is exactly that pitch pre-processes to obtain active principle asphaltene.But usual coal tar asphalt is with thick
Based on cyclophane warp, solid impurity is relatively more, and aliphatic chain is less and short, and chemical reactivity is lower;Asphalt fragrance
Spend it is lower than coal tar asphalt, but it is equally more containing solid impurity, thus obtain active principle asphaltene precondition the
One step is exactly to filter out various disposably insoluble points, including the solid impurities such as free carbon, minerals, carbon black and quinoline insolubles
(QI).
For many years, people have carried out a large amount of research filtering out various disposable indissolvable components, also develop many physics
Isolation technics and device.Method used by purifying pitch raw material PRODUCTION TRAITS respectively has its advantage and disadvantage both at home and abroad at present: (1) quiet
It is small to set sedimentation separation equipment investment, simple process, but its clean-up effect is undesirable;(2) high temperature is centrifugated good purification,
But investment is big, and equipment operating cost is high, and treating capacity is small;(3) solvent processing investment is small, and clean-up effect is preferable, but solvent is used
Amount is big, and purifying pitch yield is low, and process energy consumption is high.(4) supercriticality can be such that the viscosity of solvent, density significantly reduces, from
And accelerate QI particle to settle and removing, but this technological temperature is high, pressure is big, inflammable and explosive, industrially enforcement difficulty is very
Greatly.(5) thermosol filtration, purification effect is preferable, and technique is simpler, but requires strainer harsh, palpus pressurized treatments, operating cost
It is high;
The present invention is directed to the shortcomings that various isolation technics and device, develops a kind of solvent thermosol isolation technics and device, the skill
Art is not only provided simultaneously with thermosol filtering and solvent treatment and purification effect is good, but also the device is boosted certainly by solvent and collects solvent
It is recovered in one, can greatly reduce operating cost, difference report has been not found through retrieval.
Summary of the invention
The object of the present invention is to provide it is a kind of investment it is small, simple process, operating cost is low, the asphalt high-temperature of good purification
The method and device of extraction heat.
The method of asphalt high-temperature extraction heat of the invention, includes the following steps:
(1) preparation of sample:
Sample to be extracted is crushed to≤80 mesh on pulverizer, to realize that solvent can be sufficiently mixed with sample, when shortening extraction
Between;
(2) preparation before extracting:
The stainless steel filter plate that selected aperture is 1-13 μm is mounted in the second autoclave (15), and by the first autoclave (5), second is high
Kettle (15) and third autoclave (24) sealing are pressed, 0.6MPa pressure N is filled with2After the air-tightness for examining whole device, put by first
Stomata (9) nitrogen leak;Then by by conduction oil by the first expansion drum (10), the second expansion drum (36) and third expansion drum (28)
It is added, concurrently sets the first autoclave (5), the temperature of the second autoclave (15) and third autoclave (24) is respectively 60-140
DEG C, 60-140 DEG C, 70-120 DEG C;
(3) will it is broken after sample to be extracted and solvent by 100g:400-1000mL ratio mixing, by feed inlet (2) addition the
One autoclave (5), while the first single head heating tube (11) of the first autoclave (5) external primary heater (6) is opened, second is high
The single head heating tube (35) of kettle (15) and the single head heating tube (27) of third autoclave (24) are pressed, the first magnetic stirring apparatus is opened
(1) and the second magnetic stirring apparatus (19), revolving speed (r0) it is respectively 80-400 revs/min, 80-200 revs/min, when first high
After pressure kettle (5), the second autoclave (15) and third autoclave (24) temperature reach established temperature, by pressure gauge (39) record first
Autoclave (5) pressure, constant temperature extracting 30-100 minutes, so that pitch is completely dissolved;
(4) connection the first ball valve (8) and the second ball valve (18) and the 6th ball valve (40), the material in the first autoclave (5) are opened
Since pressure difference enters the second autoclave (15), enter in third autoclave (24) through filter plate (13) filtered filtrate, it is molten
Agent gas enters after condenser (33) condensed from the second air vent (38) and third air vent (34), into solvent recovery tank
(30), when on the first autoclave (5) pressure gauge (39) show pressure it is constant, while observe third autoclave (24) kettle top heat
Galvanic couple (31) displays temperature after being then cooled to room temperature, illustrates that solvent has been recycled to solvent completely and has returned when it peaks
Closed cans (30);
(5) solvent recovery tank (30) bottom ball valve (29) are opened and collects solvent;
(6) opening third autoclave (24) bottom valve (26) collection extraction product can lead to when the more sticky not easily collecting of product
The first air vent (9) crossed in the first autoclave (5) is filled with 0.1-0.2MPa N2, pressurizeing, which makes to extract product, quickly collects;
It (7), can be by both on fresh bitumen and solvent recovery tank (30) recovered solvent and addition part after above-mentioned steps complete (1)-(4)
After fresh solvent is according to the ratio mixing of step (3), repeatable above step (3)-step (6) is repeatedly extracted;
(8) after collecting extract, all heating systems are closed.
Extraction yield y of the present invention is calculated by following formula:
(1)
Wherein M0The weight of sample, M are extracted after broken1For the weight of all samples on filter plate (13).
Recycling design is mixed with both on fresh bitumen with same ratio, is continuously added, is repeated the above steps by feed inlet (2)
When.
Total extraction yield of extraction n times is calculated by following formula:
(2)
Wherein M0The weight of sample, M are extracted after being crushed when using for the first time for solvent01-M0nIt is broken when being reused for 1-n solvent
The weight of extraction sample, M after broken1For the weight of all samples on filter plate (13).
Extraction equipment is devised to complete the present invention, extraction equipment of the invention includes reactor, condenser pipe (33), solvent
Collecting tank (30) and controller (37), reactor is by the first autoclave (5), the second autoclave (15) and the second autoclave (24) group
At there is the first magnetic stirring apparatus 1 in, the first autoclave (5), there is a primary heater 6 in outside, and there is a first charging aperture 2 on top, and first
Temperature thermocouple 4 and the first air vent 9, upper outside are connected with the first expansion drum 10, and there is the first discharge port 7 in bottom end;Second is high
There is stainless steel filter plate 13 in pressure kettle (15), second charging aperture 12 and the second air vent 38 are arranged at top, and there is secondary heater 16 in outside,
There is the second discharge port 17 in bottom end, and upper outside is connected with the second expansion drum 36;There is the second magnetic agitation in third autoclave (24)
Device 19, top have third feed inlet 20, the second temperature thermocouple 21 and third air vent 34, outside to have third heater 23, bottom
There is third discharge port 25 at end, and upper outside is connected with third expansion drum 28;First discharge port 7 passes through first with second charging aperture 12
Ball valve 8 connects, and the second discharge port 17 is connect with third feed inlet 20 by the second ball valve 18, third discharge port 25 and third ball valve
26 connections, the second air vent 38 are connect by the 6th ball valve 40 with third air vent 34, and third air vent 34 passes through the 4th ball valve
32 connect with condenser (33), and condenser (33) is connect with solvent recovery tank (30), the first temperature thermocouple 4, the second thermometric heat
Galvanic couple 21, the first magnetic stirring apparatus 1, the second magnetic stirring apparatus 19, the first external heater 6, the second external heater 16 and
Three external heaters 23 are connected by cable with controller (37).
All connecting pipelines of the present invention are provided with heating tape and keep the temperature.Heating tape is connected with controller (37).
First external heater (6), the second external heater (16) and third external heater (23) are collet knots
Structure, and divide in each collet and the first single head heating tube 11 is separately housed, the second single head heating tube 35, third single head heating tube 27,
Used medium is conduction oil, operating temperature 25-250 in colletoC, temperature-controlled precision 1oC, temperature control use PID control
Technology, controls heating tube by controller, carries out temperature control to collet.
The filter plate (13) is stainless steel filter plate, and stainless steel filter plate (13) is 1-5 layers.Aperture is 1-13 μm.
First autoclave (5), the second autoclave (15), the second autoclave (24) and solvent recovery tank (30),
Material is 304 stainless steels, highest pressure 1MPa.
Thermosol extracting process and device provided by the present invention, also can be widely used to other field, and such as other liquid are molten
The extraction and separation of agent and solid matter.
The invention has the following advantages that
1) primary property the removing of quinoline insolubles and the recycling of solvent in pitch can be completed in one set of instrument, compared with existing
Thermosol technology is easier, fast, environmental protection.
2) it cannot be only used for liquid-solid extraction, can also be used separately as solvent distillation recovery device.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of extraction equipment of the present invention.
As shown, the 1, first magnetic stirring apparatus;2, first charging aperture;3, the first bolt;4, thermometric thermoelectricity in the first kettle
It is even;5, the first autoclave;6, primary heater;7, the first discharge port;8, the first ball valve;9, the first air vent;10, the first expansion
Tank;11, the first single head heating tube;12, second charging aperture;13, filter plate;14, the second bolt;15, the second autoclave;16, second
Heater;17, the second discharge port;18, the second ball valve;19, the second magnetic stirring apparatus;20, third feed inlet;21, in the second kettle
Temperature thermocouple;22, third bolt;23, third heater;24, third autoclave;25, third discharge port;26, third ball valve;
27, third single head heating tube;28, third expansion drum;29, the 5th ball valve;30, solvent recovery tank;31, kettle top thermocouple;32,
Four ball valves;33, condenser;34, third air vent;35, the second single head heating tube;36, second expansion drum is led;37, controller;
38, the second air vent;39, pressure gauge;40, the 6th ball valve.
Specific embodiment
Further narration in detail is done to a specific embodiment of the invention below with reference to shown in Fig. 1.
Embodiment 1
Extraction equipment of the invention includes reactor, condenser pipe (33), solvent collecting tank (30) and controller (37), reactor by
First autoclave (5), the second autoclave (15) and the second autoclave (24) composition, the first autoclave (5) is interior to have the first magnetic force to stir
Mix device 1, there is a primary heater 6 in outside, and there are first charging aperture 2, the first temperature thermocouple 4 and the first air vent 9 in top, outside top
Side is connected with the first expansion drum 10, and there is the first discharge port 7 in bottom end;There is stainless steel filter plate 13 in second autoclave (15), top has
There is secondary heater 16 in second charging aperture 12 and the second air vent 38, outside, and there are the second discharge port 17, upper outside connection in bottom end
There is the second expansion drum 36;There is the second magnetic stirring apparatus 19 in third autoclave (24), third feed inlet 20, the second thermometric are arranged at top
There is third heater 23 in thermocouple 21 and third air vent 34, outside, and there is third discharge port 25 in bottom end, and upper outside is connected with
Three expansion drums 28;First discharge port 7 is connect with second charging aperture 12 by the first ball valve 8, and the second discharge port 17 is fed with third
Mouth 20 is connected by the second ball valve 18, and third discharge port 25 is connect with third ball valve 26, and the second air vent 38 passes through the 6th ball valve
40 connect with third air vent 34, and third air vent 34 is connect by the 4th ball valve 32 with condenser (33), condenser (33) and
Solvent recovery tank (30) connection, the first temperature thermocouple 4, the second temperature thermocouple 21, the first magnetic stirring apparatus 1, the second magnetic force
Blender 19, the first external heater 6, the second external heater 16 and third external heater 23 pass through cable and controller
(37) it is connected.
All connecting pipelines are provided with heating tape and are kept the temperature.Heating tape is connected with controller (37).
First external heater (6), the second external heater (16) and third external heater (23) are collet knots
Structure, and divide in each collet and the first single head heating tube 11 is separately housed, the second single head heating tube 35, third single head heating tube 27,
Used medium is conduction oil, operating temperature 250 in colletoC, temperature-controlled precision 1oC, temperature control use PID control skill
Art, controls heating tube by controller, carries out temperature control to collet.
The filter plate 13 is stainless steel filter plate, and stainless steel filter plate 13 is 3 layers, and filter plate aperture is respectively 10 μ from top to bottom
M, 5 μm and 2 μm.
First autoclave (5), the second autoclave (15), the second autoclave (24) and solvent recovery tank (30),
Material is 304 stainless steels, and pressure resistance is 1MPa.
Each magnetic stirring apparatus model 90ZYT102A3;Each single head heating tube is SH218V400W;
Measuring device is first attached by the present invention according to mode shown in Fig. 1, sample to be extracted is crushed on pulverizer≤
80 mesh;
1, the stainless steel filter plate m that aperture is 10 μm, 5 μm and 2 μ is mounted on from top to bottom in the second autoclave (15), by first
Autoclave (5), the second autoclave (15) and third autoclave (24) sealing, are filled with 0.6MPa pressure N2Examine the gas of whole device
Conduction oil is added by heat conduction oil tank (10), (28) and (36), concurrently sets the first autoclave (5), the second autoclave by close property
(15) and the temperature of third autoclave (24) is respectively 100 DEG C, 100 DEG C, 120 DEG C;
2, broken coal tar asphalt and solvents tetrahydrofurane are mixed in the ratio of 150g:600mL, is added by feed inlet (2)
Enter the first autoclave (5), is filled with N2After examining air-tightness, while opening the of the first autoclave (5) external primary heater (6)
One single head heating tube (11), the single head heating tube (35) of the second autoclave (15) and the single head heating tube of third autoclave (24)
(27), the first magnetic stirring apparatus (1) and the second magnetic stirring apparatus (19), revolving speed (r are opened0) it is respectively 200 revs/min, 100
Rev/min, after the first autoclave (5), the second autoclave (15) and third autoclave (24) temperature reach established temperature, by pressing
Power table (39) record the first autoclave (5) pressure, constant temperature extracting 60 minutes, so that pitch is completely dissolved;
3, open connection the first ball valve (8), the second ball valve (18) and the 6th ball valve (40), material in the first autoclave (5) by
Enter the second autoclave (15) in pressure difference, enters in third autoclave (24) through filter plate (13) filtered filtrate, solvent
Gas enters after condenser (33) condensed from the second air vent (38) and third air vent (34), into solvent recovery tank
(30), when on the first autoclave (5) pressure gauge (39) show pressure it is constant, while observe third autoclave (24) kettle top heat
Galvanic couple (31) displays temperature after being then cooled to room temperature, illustrates that solvent is recycled to solvent completely when it peaks 67 DEG C
Recycling can (30);
4, solvent recovery tank (30) bottom ball valve (29) are opened and collects solvent;
5, third autoclave (24) bottom valve (26) are opened and collect extraction product;
6, after collecting extract, all heating systems are closed.
The data measured:
T1=100oC, M0=150 g, M1=56 g, 580 mL of recycling design;
Extraction yield is calculated by formula (1) are as follows: 62.67%.
Embodiment 2
It carries out according to the method for embodiment 1, except that mixing 150g asphalt sample with 600mL toluene in step 2, step
The set temperature of first autoclave (5) in 1, the second autoclave (15) and third autoclave (24) is respectively 130 DEG C, and 130 DEG C,
150 DEG C, and kettle top thermocouple (31) the displays temperature highest point of third autoclave (24) is 111 DEG C of then coolings in step 3
To room temperature, illustrate that solvent has been recycled to solvent recovery tank (30) completely.
The data of survey:
T1=130oC, M0=150 g, M1=89 g, recycling design 580mL;
Extraction yield is calculated by formula (1) are as follows: 40.67%.
Embodiment 3
It carries out according to the method for embodiment 1, except that taking identical material 150g and recycling after the 1-3 step of completion example 1
Tetrahydrofuran, then plus the fresh tetrahydrofuran of 20mL after evenly mixing, continue the first charging aperture by the first autoclave (5)
(2) it is added, repeats (2)-(6) step of example 1.
The data measured:
T1=100oC, M0=150 g+150 g=300 g, M1=108 g, recycling tetrahydrofuran solvent are 566 mL;
Extraction yield is calculated by formula (2) are as follows: 64.00%.
Claims (5)
1. a kind of method of asphalt high-temperature extraction heat, it is characterised in that include the following steps:
(1) preparation of sample:
Sample to be extracted is crushed to≤80 mesh on pulverizer, to realize that solvent can be sufficiently mixed with sample;
(2) preparation before extracting:
Selected aperture is that 1-13 μm of stainless steel filter plate is mounted in the second autoclave, by the first autoclave, the second autoclave and
The sealing of third autoclave, is filled with 0.6MPa pressure N2After the air-tightness for examining whole device, by the first air vent nitrogen leak;So
Afterwards by conduction oil to be added by the first expansion drum, the second expansion drum and third expansion drum, the first autoclave is concurrently set, second is high
The temperature for pressing kettle and third autoclave is respectively 60-140 DEG C, 60-140 DEG C, 70-120 DEG C;
(3) sample to be extracted and solvent are mixed in the ratio of 100g:400-1000mL after will be broken, and it is high to be added first by feed inlet
Kettle is pressed, while opening the first single head heating tube of primary heater outside the first autoclave, the single head heating tube of the second autoclave
With the single head heating tube of third autoclave, opens the first magnetic stirring apparatus and the second magnetic stirring apparatus, revolving speed are respectively 80-
400 revs/min, 80-200 revs/min, when the first autoclave, the second autoclave and third autoclave temp reach established temperature
Afterwards, by pressure gauge record the first autoclave pressure, constant temperature extracting 30-100 minutes so that pitch is completely dissolved;
(4) the first ball valve of connection and the second ball valve and the 6th ball valve are opened, the material in the first autoclave is entered due to pressure difference
Second autoclave, the filtrate after filter plate enter in third autoclave, and solvent gas is put from the second air vent and third
Stomata enters after condenser condensed, into solvent recovery tank, when the pressure gauge on the first autoclave shows that pressure is constant, together
When observation third autoclave kettle top thermocouple displays temperature after being then cooled to room temperature, illustrate molten when it peaks
Agent is recycled to solvent recovery tank completely;
(5) it opens solvent recovery pot bottom ball valve and collects solvent;
(6) opening third autoclave base valve collection extraction product can be by first when the more sticky not easily collecting of product
First air vent of autoclave is filled with 0.1-0.2MPa N2, pressurizeing, which makes to extract product, quickly collects;
It (7), can be fresh by both on fresh bitumen and solvent recovery tank recovered solvent and addition part after above-mentioned steps complete (1)-(4)
After solvent is according to the ratio mixing of step (3), repeatable above step (3)-step (6) is repeatedly extracted;
(8) after collecting extract, all heating systems are closed.
2. a kind of extraction equipment, it includes reactor, condenser pipe (33), solvent collecting tank (30) and controller (37), feature
It is reactor by the first autoclave (5), the second autoclave (15) and the second autoclave (24) composition, the first autoclave (5) are interior
Have the first magnetic stirring apparatus (1), outside has primary heater (6), and top has first charging aperture (2), the first temperature thermocouple (4)
With the first air vent (9), upper outside is connected with the first expansion drum (10), and bottom end has the first discharge port (7);Second autoclave
(15) have stainless steel filter plate (13) in, second charging aperture (12) and the second air vent (38) are arranged at top, and there is secondary heater in outside
(16), bottom end has the second discharge port (17), and upper outside is connected with the second expansion drum (36);Have second in third autoclave (24)
Third feed inlet (20), the second temperature thermocouple (21) and third air vent (34) are arranged at magnetic stirring apparatus (19), top, and outside has
Third heater (23), bottom end have third discharge port (25), and upper outside is connected with third expansion drum (28);First discharge port
(7) it is connect with second charging aperture (12) by the first ball valve (8), the second discharge port (17) and third feed inlet (20) pass through second
Ball valve (18) connection, third discharge port (25) are connect with third ball valve (26), and the second air vent (38) passes through the 6th ball valve (40)
It is connect with third air vent (34), third air vent (34) is connect by the 4th ball valve 32 with condenser (33), condenser (33)
It is connect with solvent recovery tank (30), the first temperature thermocouple (4), the second temperature thermocouple (21), the first magnetic stirring apparatus (1),
Second magnetic stirring apparatus (19), the first external heater (6), the second external heater (16) and third external heater (23) are equal
It is connected by cable with controller (37).
3. a kind of extraction equipment as described in claim 1, it is characterised in that all connecting pipelines are provided with heating tape progress
Heat preservation, heating tape is connected with controller (37).
4. a kind of extraction equipment as described in claim 1, it is characterised in that first external heater (6), outside second
Heater (16) and third external heater (23) are jacket structured, and divide in each collet and the first single head heating tube is separately housed
(11), the second single head heating tube (35), third single head heating tube (27), used medium is conduction oil, operating temperature in collet
For 25-250oC, temperature-controlled precision 1oC, temperature control use PID control technology, heating tube are controlled by controller (37), to folder
Pack into trip temperature control.
5. a kind of extraction equipment as described in claim 1, it is characterised in that the filter plate (13) is stainless steel filter plate, stainless
Steel filter plate (13) is 1-5 layers, and aperture is 1-13 μm.
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Cited By (2)
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CN110628448A (en) * | 2019-11-05 | 2019-12-31 | 中国矿业大学(北京) | Method and system for removing quinoline insoluble substances in coal tar pitch |
CN114874799A (en) * | 2022-06-13 | 2022-08-09 | 中国科学院山西煤炭化学研究所 | Method and device for filtering asphalt by continuous high-temperature thermal extraction |
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