CN115404092A - Method and device for continuously preparing mesophase pitch - Google Patents
Method and device for continuously preparing mesophase pitch Download PDFInfo
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- CN115404092A CN115404092A CN202211176535.5A CN202211176535A CN115404092A CN 115404092 A CN115404092 A CN 115404092A CN 202211176535 A CN202211176535 A CN 202211176535A CN 115404092 A CN115404092 A CN 115404092A
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- mixing kettle
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- 239000011302 mesophase pitch Substances 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 65
- 230000008020 evaporation Effects 0.000 claims abstract description 36
- 238000001704 evaporation Methods 0.000 claims abstract description 36
- 239000011301 petroleum pitch Substances 0.000 claims abstract description 13
- 239000011300 coal pitch Substances 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- 239000002904 solvent Substances 0.000 claims abstract description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 4
- 239000001257 hydrogen Substances 0.000 claims abstract description 4
- 239000000155 melt Substances 0.000 claims abstract description 4
- 239000010426 asphalt Substances 0.000 claims description 18
- 238000004821 distillation Methods 0.000 claims description 14
- 239000000852 hydrogen donor Substances 0.000 claims description 7
- 239000000945 filler Substances 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 5
- CXWXQJXEFPUFDZ-UHFFFAOYSA-N tetralin Chemical group C1=CC=C2CCCCC2=C1 CXWXQJXEFPUFDZ-UHFFFAOYSA-N 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 239000003245 coal Substances 0.000 claims description 3
- 239000004020 conductor Substances 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000003208 petroleum Substances 0.000 claims description 2
- 230000014759 maintenance of location Effects 0.000 claims 2
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 238000009826 distribution Methods 0.000 abstract description 5
- 238000002844 melting Methods 0.000 abstract 1
- 230000008018 melting Effects 0.000 abstract 1
- 238000000465 moulding Methods 0.000 abstract 1
- 239000011318 synthetic pitch Substances 0.000 abstract 1
- 238000006116 polymerization reaction Methods 0.000 description 7
- 239000011317 mixed pitch Substances 0.000 description 6
- 229920000049 Carbon (fiber) Polymers 0.000 description 5
- 239000004917 carbon fiber Substances 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- 239000011295 pitch Substances 0.000 description 4
- 238000006068 polycondensation reaction Methods 0.000 description 4
- 238000003763 carbonization Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 125000003118 aryl group Chemical group 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000011294 coal tar pitch Substances 0.000 description 2
- 238000005984 hydrogenation reaction Methods 0.000 description 2
- 150000002605 large molecules Chemical class 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000002841 Lewis acid Substances 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 125000000753 cycloalkyl group Chemical group 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 150000007517 lewis acids Chemical class 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000002074 melt spinning Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Images
Classifications
-
- 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
- C10C3/02—Working-up pitch, asphalt, bitumen by chemical means reaction
-
- 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
- C10C3/06—Working-up pitch, asphalt, bitumen by distillation
Abstract
The invention discloses a method and a device for continuously preparing mesophase pitch, and belongs to the technical field of synthetic pitch preparation methods. To the big problem of conventional kettle-type reactor backmixing, designed a device of continuous preparation mesophase pitch, included: mixing kettle, tubular reactor, flash evaporation kettle, constant pressure system and forming machine. Melting and mixing the crushed refined coal pitch and petroleum pitch in proportion, reacting for a certain time by a melt pump through a tubular reactor, flashing to obtain light components, then quantitatively adding a hydrogen supply solvent, continuously reacting for a certain time by the melt pump through the tubular reactor, flashing to obtain the light components, and molding to obtain the mesophase pitch. The invention adopts the tubular reactor to co-carbonize refined coal pitch and petroleum pitch, the whole reaction system has no back mixing, can control temperature by sections, has high thermal efficiency, and can continuously prepare spinnable mesophase pitch with uniform molecular weight distribution, good flowing property and moderate softening point.
Description
Technical Field
The invention belongs to the technical field of synthetic asphalt preparation methods, and particularly relates to a method and a device for continuously preparing mesophase asphalt.
Background
The high-performance pitch carbon fiber has excellent performances of high strength, high modulus, high temperature resistance, corrosion resistance, fatigue resistance, electric conduction, heat conduction and the like, is an indispensable engineering material in the aerospace industry, and is widely applied to the aspects of traffic, machinery, sports and entertainment.
The production of high-performance pitch carbon fiber relates to five process units, namely raw material refining, thermal polycondensation, melt spinning, pre-oxidation and carbonization/graphitization. The preparation of mesophase spinnable pitch by thermal polycondensation is a key step in the preparation of pitch carbon fibers. It is generally believed that good mesophase structure requires good aromatic ring molecular flatness, contains certain short alkyl and cycloalkyl structures and a concentrated molecular weight distribution. The viscosity of the system is low during the polycondensation process, so that the growth, flow and fusion of mesophase liquid crystal are ensured, and the polycondensation reaction system is required to be carried out mildly in order to avoid the formation of overlarge infusible asphalt molecules. The mesophase pitch is generally prepared by catalytic polymerization, hydrogenation-modified polymerization and co-carbonization. Catalytic polymerization is typically carried out using Lewis acid metal catalysts and HF/BF3. The metal catalyst (AlCl 3 of Japanese patent laid-open No. 61-83317) can remain in the spinnable asphalt and is difficult to completely remove, and the performance of the final carbon fiber is greatly influenced; the reaction system of HF/BF3 catalyst (Japanese patent laid-open Nos. Hei 1-139621, hei 1-254796, CN200910064562, CN 106497591B, CN 106350088B) has great corrosiveness to equipment, and has raised higher requirements for equipment. The hydrogenation modification polymerization needs to introduce aliphatic hydrogen and naphthenic structures into raw material asphalt molecules under the action of a Ni-Mo-Al2O3 catalyst under high temperature and high pressure (preparation and performance research of hydrogenated coal asphalt-based carbon fibers, wang Yuanhua, a doctor's academic paper), but the operation pressure of the hydrogenation modification polymerization reaches 16MPa, and higher requirements are also provided for equipment. Co-carbonization is a relatively ideal method for producing mesophase pitch, and mesophase pitch having excellent properties can be produced by introducing the fatty structure in petroleum pitch into the high aromatic ring structure of coal pitch by polymerization. (Guo J, et al., energy Fuels2020,34, 6474-6482). However, a tank reactor is usually used for preparing the mesophase pitch, back mixing is large, and polymerization reaction between small molecules and between large molecules and large molecules is easy to occur, so that the molecular weight distribution of the generated mesophase pitch is wide, and the performance of the mesophase pitch is influenced.
Disclosure of Invention
Aiming at the problem of large back mixing of a conventional kettle type reactor, the invention provides a method and a device for continuously preparing mesophase pitch.
In order to achieve the purpose, the invention adopts the following technical scheme:
an apparatus for continuously preparing mesophase pitch comprising: a mixing kettle, a tubular reactor, a flash evaporation kettle, a constant pressure system and a forming machine;
the mixing kettle comprises a first mixing kettle and a second mixing kettle; the tubular reactor comprises a first tubular reactor and a second tubular reactor; the flash evaporation kettle comprises a first flash evaporation kettle and a second flash evaporation kettle; the constant pressure system comprises a first constant pressure system and a second constant pressure system;
the first mixing kettle is provided with a first magnetic stirrer, the outer side of the first mixing kettle is provided with a heater, the top end of the first mixing kettle is provided with a first feeding hole and a second feeding hole, and the bottom end of the first mixing kettle is provided with a first discharging hole; the second mixing kettle is provided with a second magnetic stirrer, the outer side of the second mixing kettle is provided with a heater, the top end of the second mixing kettle is provided with a third feeding system, and the bottom end of the second mixing kettle is provided with a third discharge hole; heaters are arranged on the outer sides of the first tubular reactor and the second tubular reactor, heat-conducting fillers are arranged in the middle of the tubes, and the fillers are graphite particles or aluminum particle heat conductors; heaters are arranged on the outer sides of the first flash evaporation kettle and the second flash evaporation kettle respectively, the top ends of the first flash evaporation kettle and the second flash evaporation kettle are respectively provided with a first distillation outlet and a second distillation outlet, and the bottom ends of the first flash evaporation kettle and the second flash evaporation kettle are respectively provided with a second discharge hole and a fourth discharge hole;
the first discharge hole is connected with the inlet of a first melt pump through a valve, and the outlet of the first melt pump is connected with the inlet of the first tubular reactor; the outlet of the first tubular reactor is connected with a first flash evaporation kettle through a first constant pressure system, and the first distillation outlet is connected with a first vacuum pump through a valve; the second discharge port is connected with the inlet of a second melt pump through a one-way valve and a stainless steel pipe, and the outlet of the second melt pump is connected with a second mixing kettle; the third discharge hole is connected with the inlet of a third melt pump through a valve, and the outlet of the third melt pump is connected with the inlet of the second tubular reactor; the outlet of the second tubular reactor is connected with a second flash evaporation kettle through a second constant pressure system, and the second distillation outlet is connected with a second vacuum pump through a valve; the fourth discharge port is connected with the inlet of the fourth melt pump through a one-way valve and a stainless steel pipe, and the outlet of the fourth melt pump is connected with a forming machine.
A method for preparing mesophase pitch by using the continuous mesophase pitch preparation device comprises the following steps:
step 1, sample preparation: respectively crushing the refined coal pitch and the petroleum pitch on a crusher to be less than or equal to 60 meshes;
And 3, obtaining the product at the outlet of the forming machine, namely the mesophase pitch.
Further, the working temperatures of the first mixing kettle and the second mixing kettle are 160-180 ℃ and 420-450 ℃ respectively.
Further, the rotating speeds of the first magnetic stirrer and the second magnetic stirrer are 150-200 revolutions per minute.
Further, the working temperatures of the first tubular reactor and the second tubular reactor are respectively 420-450 ℃ and 400-420 ℃, and the temperature of the forming machine is 320-350 ℃.
Further, the set pressures of the first low-pressure system and the second low-pressure system are respectively 3-5 MPa and 2-3 MPa.
Further, the mixing ratio of the crushed coal asphalt and the crushed petroleum asphalt is 1:1-3:1.
Furthermore, the hydrogen donor solvent is tetrahydronaphthalene, and the addition amount of the hydrogen donor solvent is 5-10% of the flow of the asphalt at the outlet of the melt pump.
Further, the residence time of the mixed asphalt in the first tubular reactor is 6-8 h, and the residence time of the mixed asphalt in the second tubular reactor is 4-6 h.
Further, the length of the first tubular reactor and the length of the second tubular reactor are both 80m, and the pipe diameter is both 50mm.
Compared with the prior art, the invention has the following advantages:
the method and the device for continuously preparing the mesophase pitch adopt a mode of the plug flow of the tubular reactor, solve the problem of large back mixing of the conventional kettle type reactor, can continuously feed and discharge materials, greatly improve the production efficiency, ensure uniform temperature of the whole reaction system, and realize the preparation of the spinnable mesophase pitch with uniform molecular weight distribution, moderate softening point and good flow property on one set of instruments.
Drawings
FIG. 1 is a schematic diagram of the structure of an apparatus for producing mesophase pitch according to the present invention;
FIG. 2 is a graph of the molecular weight distribution of mesophase pitch made according to the present invention;
FIG. 3 is a graph of the flow properties of mesophase pitch made according to the present invention.
Reference numerals: 1. a first magnetic stirrer; 2. a first feed port; 3. a first mixing kettle; 4. a first discharge port; 5. a first melt pump; 6. a second melt pump; 7. a second mixing kettle; 8. a third melt pump; 9. a second feed port; 10. a first tubular reactor; 11. a first constant pressure system; 12. a first vacuum pump; 13. a first distillation outlet; 14. a first flash kettle; 15. a second discharge port; 16. a first check valve; 17. a second magnetic stirrer; 18. a feed system; 19. a third discharge port; 20. a second tubular reactor; 21. a second constant pressure system; 22. a second vacuum pump; 23. a second distillation outlet; 24. a second flash evaporation kettle; 25. a fourth discharge port; 26. a fourth melt pump; 27. a forming machine; 28. a second one-way valve.
Detailed Description
Example 1
An apparatus for continuously producing mesophase pitch comprising: a mixing kettle, a tubular reactor, a flash evaporation kettle, a constant pressure system and a forming machine 27;
the mixing kettle comprises a first mixing kettle 3 and a second mixing kettle 7; the tubular reactor comprises a first tubular reactor 10 and a second tubular reactor 20; the flash tank comprises a first flash tank 14 and a second flash tank 24; the constant pressure system comprises a first constant pressure system 11 and a second constant pressure system 21;
the first mixing kettle 3 is provided with a first magnetic stirrer 1, the outer side of the first mixing kettle is provided with a heater, the top end of the first mixing kettle is provided with a first feeding hole 2 and a second feeding hole 9, and the bottom end of the first mixing kettle is provided with a first discharging hole 4; the second mixing kettle 7 is provided with a second magnetic stirrer 17, the outer side of the second mixing kettle is provided with a heater, the top end of the second mixing kettle is provided with a third feeding system 18, and the bottom end of the second mixing kettle is provided with a third discharging hole 19; heaters are arranged on the outer sides of the first tubular reactor 10 and the second tubular reactor 20, heat-conducting fillers are arranged in the middle of the tubes, and the fillers are graphite particles or aluminum particle heat conductors; the outer sides of the first flash evaporation kettle 14 and the second flash evaporation kettle 24 are respectively provided with a heater, the top ends of the first flash evaporation kettle and the second flash evaporation kettle are respectively provided with a first distillation outlet 13 and a second distillation outlet 23, and the bottom ends of the first flash evaporation kettle and the second flash evaporation kettle are respectively provided with a second discharge hole 15 and a fourth discharge hole 25;
the first discharge port 4 is connected with an inlet of a first melt pump 5 through a valve, and an outlet of the first melt pump 5 is connected with an inlet of a first tubular reactor 10; an outlet of the first tubular reactor 10 is connected with a first flash kettle 14 through a first constant pressure system 11, and a first distillation outlet 13 is connected with a first vacuum pump 12 through a valve; the second discharge port 15 is connected with the inlet of the second melt pump 6 through a one-way valve 16 by a stainless steel pipe, and the outlet of the second melt pump 6 is connected with the second mixing kettle 7; the third discharge port 19 is connected with the inlet of the third melt pump 8 through a valve, and the outlet of the third melt pump 8 is connected with the inlet of the second tubular reactor 20; an outlet of the second tubular reactor 20 is connected with a second flash evaporation kettle 24 through a second constant pressure system 21, and a second distillation outlet 23 is connected with a second vacuum pump 22 through a valve; the fourth discharge port 25 is connected with the inlet of a fourth melt pump 26 through a one-way valve 28 by a stainless steel pipe, and the outlet of the fourth melt pump 26 is connected with a forming machine 27.
Example 2
Firstly, connecting the reaction device of the embodiment 1 according to the mode shown in the figure 1, and crushing the refined coal pitch and the petroleum pitch on a crusher to be less than or equal to 60 meshes;
continuously adding the crushed sample into a first mixing kettle 3 from a first feed port 2 and a second feed port 9 according to the proportion of coal pitch to petroleum pitch (weight ratio) of 1:1, simultaneously starting an external heater of the first mixing kettle 3, setting the temperature to be 160 ℃, starting a first magnetic stirrer 1, setting the rotating speed to be 150 r/min, simultaneously starting a first melt pump 5, setting the flow rate to ensure that the residence time of the first melt pump in a tubular reactor with the diameter of 50mm and the length of 80m is 6h, simultaneously starting heaters of a first tubular reactor 10 and a second tubular reactor 20, setting the temperatures to be 450 ℃ and 420 ℃, starting heaters of a first flash evaporation kettle 14 and a second flash evaporation kettle 24, setting the temperatures to be 420 ℃ and 400 ℃, the vacuum degrees to be-0.09 MPa (gauge pressure), setting the pressures of a first constant pressure system 11 and a second constant pressure system 21 to be 3MPa and 2MPa, and setting the temperature of a forming machine 27 to be 320 MPa; after the coal pitch and the petroleum pitch are mixed for 10min at 180 ℃, the first melt pump 5 is started, when the mixed pitch reaches the outlet of the first tubular reactor 10, the second melt pump 6 and the third melt pump 8 are started, the flow rate is set, the residence time of the mixed pitch in the second tubular reactor 20 with the diameter of 60mm and the length of 80m is 4h, the third feeding system 18 is simultaneously started, the hydrogen donor tetrahydronaphthalene is added according to 5% of the flow rate of the second melt pump 6, when the mixture reaches the outlet of the second tubular reactor 20, the fourth melt pump 26 and the forming machine 27 are started, and the product at the outlet of the forming machine 27 is the mesophase pitch with the softening point of 270 ℃.
Example 3
Firstly, connecting the reaction device of the embodiment 1 according to the mode shown in figure 1, and crushing refined coal pitch and petroleum pitch on a crusher to be less than or equal to 60 meshes;
continuously adding the crushed sample into a first mixing kettle 3 from a first feeding hole 2 and a second feeding hole 9 according to the weight ratio of coal tar pitch to petroleum pitch (2:1), simultaneously starting an external heater of the first mixing kettle 3, setting the temperature to be 180 ℃, starting a first magnetic stirrer 1, setting the rotating speed to be 170 rpm, simultaneously starting a first melt pump 5, setting the flow rate to ensure that the residence time of the first melt pump in a tubular reactor with the diameter of 60mm and the length of 80m is 7h, simultaneously starting heaters of a first tubular reactor 10 and a second tubular reactor 20, setting the temperatures to be 430 ℃ and 400 ℃, starting heaters of a first flash evaporation kettle 14 and a second flash evaporation kettle 24, setting the temperatures to be 400 ℃ and 380 ℃, setting the vacuum degrees to be-0.09 (gauge pressure), setting the pressures of a first constant pressure system 11 and a second constant pressure system 21 to be 5MPa and 3 respectively, and setting the temperature of a forming machine 27 to be 350 MPa; after the coal pitch and the petroleum pitch are mixed for 10min at 180 ℃, the first melt pump 5 is started, when the mixed pitch reaches the outlet of the first tubular reactor 10, the second melt pump 6 and the third melt pump 8 are started, the flow rate is set, the residence time of the mixed pitch in the second tubular reactor 20 with the diameter of 60mm and the length of 80m is 5h, the third feeding system 18 is simultaneously started, the hydrogen donor tetrahydronaphthalene is added according to 7% of the flow rate of the second melt pump 6, when the mixture reaches the outlet of the second tubular reactor 20, the fourth melt pump 26 and the forming machine 27 are started, and the product at the outlet of the forming machine 27 is the mesophase pitch with the softening point of 295 ℃.
Example 4
Continuously adding the crushed sample into a first mixing kettle 3 through a first feeding hole 2 and a second feeding hole 9 according to the proportion of coal tar pitch and petroleum pitch (weight ratio) of 3:1, simultaneously starting an external heater of the first mixing kettle 3, setting the temperature to be 170 ℃, starting a first magnetic stirrer 1, setting the rotating speed to be 200 r/min, simultaneously starting a first melt pump 5, setting the flow rate to enable the residence time of the first melt pump to be 8h in a tubular reactor with the diameter of 60mm and the length of 80m, simultaneously starting heaters of a first tubular reactor 10 and a second tubular reactor 20, setting the temperatures to be 420 ℃ and 410 ℃, starting heaters of a first flash evaporation kettle 14 and a second flash evaporation kettle 24, setting the temperatures to be 410 ℃ and 390 MPa, setting the vacuum degree to be-0.09 (gauge pressure), setting the pressures of a first constant pressure system 11 and a second constant pressure system 21 to be 4MPa and 2 respectively, and setting the temperature of a forming machine 27 to be 330 MPa; after the coal pitch and the petroleum pitch are mixed for 10min at 170 ℃, the first melt pump 5 is started, when the mixed pitch reaches the outlet of the first tubular reactor 10, the second melt pump 6 and the third melt pump 8 are started, the flow rate is set, the residence time of the mixed pitch in the second tubular reactor 20 with the diameter of 60mm and the length of 80m is 6h, the third feeding system 18 is simultaneously started, the hydrogen donor tetrahydronaphthalene is added according to 10 percent of the flow rate of the second melt pump 6, when the mixture reaches the outlet of the second tubular reactor 20, the fourth melt pump 26 and the forming machine 27 are started, and the product at the outlet of the forming machine 27 is the mesophase pitch with the softening point of 280 ℃.
Those matters not described in detail in the present specification are well known in the art to which the skilled person pertains. Although illustrative embodiments of the present invention have been described above to facilitate the understanding of the present invention by those skilled in the art, it should be understood that the present invention is not limited to the scope of the embodiments, and various changes may be made apparent to those skilled in the art as long as they are within the spirit and scope of the present invention as defined and defined by the appended claims, and all matters of the invention which utilize the inventive concepts are protected.
Claims (10)
1. An apparatus for continuously preparing mesophase pitch, characterized in that: the method comprises the following steps: a mixing kettle, a tubular reactor, a flash evaporation kettle, a constant pressure system and a forming machine (27);
the mixing kettle comprises a first mixing kettle (3) and a second mixing kettle (7); the tubular reactor comprises a first tubular reactor (10) and a second tubular reactor (20); the flash tank comprises a first flash tank (14) and a second flash tank (24); the constant pressure system comprises a first constant pressure system (11) and a second constant pressure system (21);
the first mixing kettle (3) is provided with a first magnetic stirrer (1), the outer side of the first mixing kettle is provided with a heater, the top end of the first mixing kettle is provided with a first feeding hole (2) and a second feeding hole (9), and the bottom end of the first mixing kettle is provided with a first discharging hole (4); the second mixing kettle (7) is provided with a second magnetic stirrer (17), the outer side of the second mixing kettle is provided with a heater, the top end of the second mixing kettle is provided with a third feeding system (18), and the bottom end of the second mixing kettle is provided with a third discharging hole (19); heaters are arranged on the outer sides of the first tubular reactor (10) and the second tubular reactor (20), heat-conducting fillers are arranged in the middle of the tubes, and the fillers are graphite particles or aluminum particle heat conductors; heaters are respectively arranged on the outer sides of the first flash evaporation kettle (14) and the second flash evaporation kettle (24), the top ends of the heaters are respectively provided with a first distillation outlet (13) and a second distillation outlet (23), and the bottom ends of the heaters are respectively provided with a second discharge hole (15) and a fourth discharge hole (25);
the first discharge port (4) is connected with an inlet of a first melt pump (5) through a valve, and an outlet of the first melt pump (5) is connected with an inlet of a first tubular reactor (10); an outlet of the first tubular reactor (10) is connected with a first flash kettle (14) through a first constant pressure system (11), and a first distillation outlet (13) is connected with a first vacuum pump (12) through a valve; the second discharge port (15) is connected with the inlet of a second melt pump (6) through a one-way valve (16) by a stainless steel pipe, and the outlet of the second melt pump (6) is connected with a second mixing kettle (7); the third discharge hole (19) is connected with the inlet of a third melt pump (8) through a valve, and the outlet of the third melt pump (8) is connected with the inlet of a second tubular reactor (20); an outlet of the second tubular reactor (20) is connected with a second flash evaporation kettle (24) through a second constant pressure system (21), and a second distillation outlet (23) is connected with a second vacuum pump (22) through a valve; the fourth discharge port (25) is connected with the inlet of a fourth melt pump (26) through a one-way valve (28) by a stainless steel pipe, and the outlet of the fourth melt pump (26) is connected with a forming machine (27).
2. A method for preparing mesophase pitch by using the continuous mesophase pitch preparation device is characterized by comprising the following steps: the method comprises the following steps:
step 1, sample preparation: respectively crushing the refined coal pitch and the petroleum pitch on a crusher to be less than or equal to 60 meshes;
step 2, adding the crushed sample into a first mixing kettle (3) from a first feeding hole (2) and a second feeding hole (9) in proportion, simultaneously starting an external heater of the first mixing kettle (3), starting a first magnetic stirrer (1), and simultaneously setting the flow rates of a first melt pump (5) and a second melt pump (16), the temperatures of a first tubular reactor (10) and a second tubular reactor (20), the temperatures of a first flash evaporation kettle (14) and a second flash evaporation kettle (24), the pressures of a first constant pressure system (11) and a second constant pressure system (21) and the temperature of a forming machine (27); after mixing for a certain time, opening a first melt pump (5), and opening a first vacuum pump (12) and a second melt pump (6) when the mixed asphalt reaches the outlet of the first tubular reactor (10) through the flow of the first melt pump (5), the length and the pipe diameter of the first tubular reactor (10); and simultaneously setting the flow rate of the third feeding system (18), adding a hydrogen supply solvent from the third feeding system (18), and simultaneously opening the third melt pump (8), the second vacuum pump (22), the fourth melt pump (26) and the forming machine (27).
And 3, obtaining the product at the outlet of the forming machine (27) as the mesophase pitch.
3. The method of producing continuous mesophase pitch according to claim 2, characterized in that: the working temperatures of the first mixing kettle (3) and the second mixing kettle (7) are 160-180 ℃ and 420-450 ℃ respectively.
4. The method of producing continuous mesophase pitch according to claim 2, characterized in that: the rotating speeds of the first magnetic stirrer (1) and the second magnetic stirrer (17) are both 150-200 r/min.
5. The method of producing continuous mesophase pitch according to claim 2, characterized in that: the working temperatures of the first tubular reactor (10) and the second tubular reactor (20) are respectively 420-450 ℃ and 400-420 ℃, and the temperature of the forming machine (27) is 320-350 ℃.
6. The method of producing continuous mesophase pitch according to claim 2, characterized in that: the set pressures of the first low-pressure system (11) and the second low-pressure system (21) are respectively 3-5 MPa and 2-3 MPa.
7. The method of producing continuous mesophase pitch according to claim 2, characterized in that: the mixing ratio of the crushed coal asphalt and the crushed petroleum asphalt is 1:1-3:1.
8. The method of producing continuous mesophase pitch according to claim 2, characterized in that: the hydrogen donor solvent is tetrahydronaphthalene, and the addition amount of the hydrogen donor solvent is 5-10% of the flow of the asphalt at the outlet of the melt pump (6).
9. The method of producing continuous mesophase pitch according to claim 2, characterized in that: the retention time of the mixed asphalt in the first tubular reactor (10) is 6-8 h, and the retention time of the mixed asphalt in the second tubular reactor (20) is 4-6 h.
10. The method of producing continuous mesophase pitch according to claim 2, characterized in that: the length of the first tubular reactor (10) and the length of the second tubular reactor (20) are both 80m, and the pipe diameter is both 50mm.
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| CN202211176535.5A CN115404092B (en) | 2022-09-26 | Method and device for continuously preparing mesophase pitch |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN87103787A (en) * | 1986-05-26 | 1987-12-23 | 饭塚幸三 | The method for preparing mesophase pitch |
| CN1031556A (en) * | 1987-06-18 | 1989-03-08 | 丸善石油化学株式会社 | Preparation bituminous method |
| CN103965932A (en) * | 2014-04-30 | 2014-08-06 | 上海宝聚新化能源科技有限公司 | Treatment method for mixed asphalt as raw material for preparing needle coke |
| US9376626B1 (en) * | 2011-04-28 | 2016-06-28 | Advanced Carbon Products, LLC | Turbulent mesophase pitch process and products |
| CN113667505A (en) * | 2020-05-15 | 2021-11-19 | 中国石油化工股份有限公司 | Production method and production system of mesophase pitch |
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN87103787A (en) * | 1986-05-26 | 1987-12-23 | 饭塚幸三 | The method for preparing mesophase pitch |
| CN1031556A (en) * | 1987-06-18 | 1989-03-08 | 丸善石油化学株式会社 | Preparation bituminous method |
| US9376626B1 (en) * | 2011-04-28 | 2016-06-28 | Advanced Carbon Products, LLC | Turbulent mesophase pitch process and products |
| CN103965932A (en) * | 2014-04-30 | 2014-08-06 | 上海宝聚新化能源科技有限公司 | Treatment method for mixed asphalt as raw material for preparing needle coke |
| CN113667505A (en) * | 2020-05-15 | 2021-11-19 | 中国石油化工股份有限公司 | Production method and production system of mesophase pitch |
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