CN115161054B - Production method of graphite coating material - Google Patents

Production method of graphite coating material Download PDF

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CN115161054B
CN115161054B CN202211070282.3A CN202211070282A CN115161054B CN 115161054 B CN115161054 B CN 115161054B CN 202211070282 A CN202211070282 A CN 202211070282A CN 115161054 B CN115161054 B CN 115161054B
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tower
asphalt
reaction kettle
softening point
thermal polymerization
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CN115161054A (en
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王海清
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Tianjin Beihai Petrochemical Engineering Co ltd
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Tianjin Beihai Petrochemical Engineering Co ltd
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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
    • C10C3/06—Working-up pitch, asphalt, bitumen by distillation
    • 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
    • C10C3/14—Solidifying, Disintegrating, e.g. granulating
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Civil Engineering (AREA)
  • Structural Engineering (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Electrochemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Working-Up Tar And Pitch (AREA)

Abstract

The invention relates to a production method of a graphite coating material, which comprises the following steps: (1) Rectification, namely obtaining the raw material ethylene tar through two-stage rectification
Figure 674842DEST_PATH_IMAGE001
A softening point asphalt; (2) thermal polymerization: performing thermal polymerization in a two-stage reaction kettle, and adjusting the pH and the content of impurity sulfur in the thermal polymerization process; (3) short path molecular distillation; and (4) filtering and granulating. According to the invention, the ammonia phosphate is added into the second reaction kettle, so that the content of sulfur-containing impurities such as sulfur-containing heterocyclic compounds in the coating material is reduced, the phenomenon that the lithium ions react with the sulfur-containing impurities due to the overhigh sulfur-containing impurities in the coating material is avoided, the reduction of the effective lithium ion content is avoided, the electrochemical performance of the battery is enhanced, and the service life of the material is prolonged.

Description

Production method of graphite coating material
Technical Field
The invention belongs to the technical field of graphite coating materials, and particularly relates to a production method of a graphite coating material.
Background
At present, the first coulombic efficiency ICE of the commercial graphite cathode is generally
Figure DEST_PATH_IMAGE001
On the other hand, the lost part is actually a part of active lithium ions lost, and one of the losses is irreversible lithium intercalation in the negative electrode. The negative electrode is irreversibly lithium-intercalated, which means that part of active lithium ions can not be extracted after entering the carbon negative electrode. Wherein the hygroscopicity of the coating material is one of the factors affecting the lithium ion activity in the carbon negative electrode material, but the prior art is less concerned.
Through searching, the following three patent publications relevant to the patent application of the invention are found:
patent document CN112592734A discloses a continuous production method of a lithium ion battery negative electrode coating material, the invention discloses a continuous production method of a lithium ion battery negative electrode coating material, comprising the following steps: (1) preheating raw materials: preheating raw material ethylene tar or ethylene residual oil in raw oil storage tank
Figure 172049DEST_PATH_IMAGE002
The preheated raw material is conveyed to a primary condensation preheater and a raw oil preheater by using a conveying pump, and the primary condensation preheater heats the raw material to
Figure DEST_PATH_IMAGE003
The raw oil preheater heats the raw material oil to
Figure 394083DEST_PATH_IMAGE004
(ii) a (2) rectification: conveying the preheated raw materials into a rectifying tower through a conveying pump for rectifying treatment to obtain a product with a softening point less than or equal to
Figure DEST_PATH_IMAGE005
The asphalt of (a); (3) distillation: the product is conveyed into a short-path distiller by a conveying pump, and the temperature in the short-path distiller
Figure 478713DEST_PATH_IMAGE006
Absolute degree of vacuum
Figure DEST_PATH_IMAGE007
To obtain a softening point of more than
Figure 709975DEST_PATH_IMAGE008
The asphalt of (a); (4) filtering: melting and filtering the materials at high temperature, and obtaining the filtering precision
Figure DEST_PATH_IMAGE009
(ii) a And (5) granulating and storing: and (4) granulating and storing the material obtained after filtering in the step (4).
Patent document CN107163971A discloses a continuous production method of a pitch-based carbon material raw material, comprising the following steps: (1) Filtering and preheating tar serving as a raw material, and then carrying out reduced pressure distillation to obtain crude asphalt; (2) Pumping the crude asphalt obtained in the step (1) to a thermal polycondensation reaction kettle, and carrying out thermal polycondensation reaction in a vacuum state to obtain tar asphalt; (3) Conveying the tar pitch obtained in the step (2) to a wiped film evaporator through a conveying pump, and removing light components in the tar pitch again to improve the distribution of pitch components; (4) The softening point is higher than that obtained in the step (3)
Figure 563661DEST_PATH_IMAGE010
Filtering the finished product asphalt through high-temperature solution; (5) Will be step (4)And cooling and granulating the filtered product, and conveying the product to a finished product bin for storage.
Patent document CN113337304A discloses a continuous production method of graphite coating material, which provides a continuous production method of graphite coating material, comprising preheating raw oil; is conveyed to a preheater to be heated to
Figure DEST_PATH_IMAGE011
Then the raw oil is sent into a dehydrating tower to be dehydrated; then, raw oil is conveyed into a next-stage preheater, heated and subjected to first vacuum rectification, fractions are respectively conveyed to an evaporator and a reboiler through a conveying pump at the bottom of a rectifying tower kettle, the fractions obtained by rectification are respectively conveyed to the middle part of the rectifying tower and the upper part of the rectifying tower kettle, and after the second vacuum rectification, a softening point is produced
Figure 691017DEST_PATH_IMAGE012
The asphalt of (a); then conveying the asphalt into a first reaction kettle for reaction to obtain asphalt with a softening point of
Figure DEST_PATH_IMAGE013
The asphalt of (a); then conveying the mixture to a second reaction kettle for reaction to obtain a mixture with a softening point of
Figure 528523DEST_PATH_IMAGE014
The asphalt of (a); finally, the mixture is sent into two wiped film evaporators to obtain the product with the softening point of
Figure DEST_PATH_IMAGE015
The asphalt of (1).
In the manufacturing method according to the above patent document, the pH and the sulfur content of the product are not adjusted, and according to the results of the inventors' examination, the above materials are all acidic and have a high sulfur content.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provides a method for producing a graphite coating material with a product pH value of 9 and low sulfur content.
The technical scheme adopted by the invention for solving the technical problem is as follows:
a production method of a graphite coating material comprises the following steps:
(1) Rectification, namely obtaining the raw material ethylene tar through two-stage rectification
Figure 32317DEST_PATH_IMAGE016
A softening point asphalt;
(2) Heat polymerization: qualified product at the bottom of the tower
Figure 802827DEST_PATH_IMAGE016
The pitch with softening point is sent into a first reaction kettle by a pitch delivery pump for thermal polymerization, and the pitch with softening point is added in the reaction kettle in the thermal polymerization process
Figure 100002_DEST_PATH_IMAGE017
Liquid, stirring and fully contacting with asphalt until the pH value in the reaction kettle reaches
Figure 101084DEST_PATH_IMAGE018
(ii) a Maintaining the thermal polymerization temperature of the first reaction vessel
Figure 100002_DEST_PATH_IMAGE019
Operating pressure of
Figure 425886DEST_PATH_IMAGE020
The residence time is
Figure 100002_DEST_PATH_IMAGE021
；
The material discharged from the first reaction kettle enters the second reaction kettle through the delivery pump to continue thermal polymerization, and the asphalt quality is introduced during the first half hour of the thermal polymerization
Figure 733371DEST_PATH_IMAGE022
The ammonium phosphate benzene solution or the benzene suspension is heated and uniformly stirred for at least 1 hour after thermal polymerization; temperature maintenance of the second reaction vessel
Figure 92808DEST_PATH_IMAGE019
At an operating pressure of
Figure 358704DEST_PATH_IMAGE020
The total residence time is
Figure 100002_DEST_PATH_IMAGE023
；
(3) Short path molecular distillation
Conveying the asphalt thermally polymerized in the second reaction kettle to a short-path molecular distiller for processing the asphalt with a high softening point; after entering the short-path molecular distiller, the asphalt is heated by the short-path molecular distiller to vaporize light components in the asphalt, and then the light components are led out and condensed, so that the light components and the heavy components are separated; obtaining the heavy fraction
Figure 701961DEST_PATH_IMAGE024
Softening point asphalt; the operation pressure of the short-path molecular evaporator is negative pressure, and the vacuum degree is
Figure 338435DEST_PATH_IMAGE020
；
(4) Filtering and granulating
Figure 21220DEST_PATH_IMAGE024
The asphalt with softening point is input into the material through a pump for filtering, a magnetic filter is adopted for filtering, and the filtered asphalt enters a granulator for granulation.
Moreover, the rectification step is as follows: ethylene tar is preheated to the feeding temperature by a two-tower coupling preheater and a one-tower coupling preheater
Figure 100002_DEST_PATH_IMAGE025
Then enters a rectifying tower to be rectified, the rectified light component gas flows out from the top of the tower and is condensed to the bottom of the tower through a tower coupling preheater and a tower condenser
Figure 723597DEST_PATH_IMAGE026
Entering a tower reflux tank, and refluxing a part of the liquid to a towerA part of the mixture is pumped into a light oil cooler to be cooled to
Figure 100002_DEST_PATH_IMAGE027
Then entering a light oil receiving tank for temporary storage;
a circulating pump is arranged at the bottom of the tower for forced circulation, and the circulating pump returns to the bottom and the middle part of the tower again after passing through a reboiler and an evaporator; qualified product at the bottom of tower
Figure 757412DEST_PATH_IMAGE028
The softened asphalt is sent to be granulated partially through an asphalt delivery pump, and sent to a second tower of a rectifying tower for further rectification partially, and the rectified light component gas flows out from the top of the first tower and is condensed to be the asphalt in a second tower coupling preheater
Figure 100002_DEST_PATH_IMAGE029
Entering a reflux tank of the second tower, refluxing a part of the reflux liquid to the second tower, and pumping a part of the reflux liquid into a light oil cooler for cooling to
Figure 406699DEST_PATH_IMAGE027
Then entering a light oil receiving tank for temporary storage;
the bottom of the second tower is provided with a circulating pump for forced circulation, the circulating pump passes through a reboiler and an evaporator and returns to the bottom and the middle part of the tower again, and the bottom of the tower is a qualified product
Figure 740729DEST_PATH_IMAGE030
A softening point asphalt.
Furthermore, the jacket of the short-path molecular distillation device is heated by molten salt provided by a molten salt furnace, and the operating temperature is
Figure 100002_DEST_PATH_IMAGE031
。
And the light component and the heavy component enter a light component receiving tank and a heavy component receiving tank which are matched with the light component and the heavy component, and the medium in the light component receiving tank is low-softening-point asphalt which is subjected to granulation.
The invention has the advantages and positive effects that:
1. the inventionBy adding into a first reaction kettle
Figure 551690DEST_PATH_IMAGE032
Reacting until the pH value of the asphalt in the reaction kettle reaches
Figure 100002_DEST_PATH_IMAGE033
The higher the pH value, the stronger the guiding effect on the flow direction of lithium ions, the higher the initial coulomb efficiency of the coating material is, the higher the pH value, the lower the hygroscopicity of the material, the lower the expansion coefficient of the material, no influence on electron transfer and increased conductivity.
2. According to the invention, the ammonia phosphate is added into the second reaction kettle, so that the content of sulfur-containing impurities such as sulfur-containing heterocyclic compounds in the coating material is reduced, the phenomenon that the lithium ions react with the sulfur-containing impurities due to the overhigh sulfur-containing impurities in the coating material is avoided, the reduction of the effective lithium ion content is avoided, the electrochemical performance of the battery is enhanced, and the service life of the material is prolonged.
3. According to the invention
Figure 72801DEST_PATH_IMAGE024
After the asphalt with the softening point passes through the two-stage evaporator, the asphalt is filtered by the magnetic filter, heavy metal impurities are removed by filtration, the ash content of the material can be effectively reduced, and the quality and the performance of the material are further improved.
Drawings
FIG. 1 is a schematic diagram of a T101 circulation reaction in a rectifying tower of the present invention.
FIG. 2 is a schematic diagram of a second column T102 of the rectifying column of the present invention.
FIG. 3 is a drawing of the present invention
Figure 791358DEST_PATH_IMAGE034
Reaction vessel R101 and
Figure 100002_DEST_PATH_IMAGE035
reaction vessel R102 is a schematic diagram of a cyclic reaction.
FIG. 4 is a schematic diagram of a short path molecular distillation cycle reaction of the present invention.
Detailed Description
The present invention is further illustrated by the following examples, which are intended to be illustrative, not limiting and are not intended to limit the scope of the invention.
The various experimental procedures involved in the embodiments of the present invention are all conventional in the art, and those skilled in the art can refer to the various conventional tool books, scientific documents, or relevant specifications, manuals, etc. before the filing date of the present application.
The production process based on the high-softening-point asphalt mainly comprises the working procedures of rectification, thermal polymerization, short-range molecular distillation, filtration, granulation, packaging and the like, and the main process flow is briefly described as follows:
example 1:
a production method of a graphite coating material comprises the following steps:
(1) Rectification
Ethylene tar (composition table 1) was passed through an E106 two-column coupled preheater, an E101 one-column coupled preheater, an E105 preheater to feed temperature
Figure 714315DEST_PATH_IMAGE036
Then enters a rectifying tower, namely a tower T101 (the operation pressure at the top of the tower)
Figure DEST_PATH_IMAGE037
) Rectifying, and discharging the light component gas from the top of T101 tower (tower top operation temperature)
Figure 961757DEST_PATH_IMAGE038
) Condensed to a tower coupling preheater E101 and a tower condenser E102
Figure DEST_PATH_IMAGE039
Entering a tower reflux tank V101, part of the gas flows back to a tower, and part of the gas is pumped into a light oil cooler to be cooled to
Figure 766902DEST_PATH_IMAGE040
Then enters the light oil jointThe collecting tank V103 is temporarily stored.
One column bottom (operating temperature)
Figure DEST_PATH_IMAGE041
) A circulating pump P102 is arranged for forced circulation, and the circulating pump circulates through a reboiler E103 and an evaporator E104 and returns to the bottom and the middle part of the tower again. Qualified product at the bottom of tower
Figure 757992DEST_PATH_IMAGE042
The softened point pitch is sent to a second rectifying tower T102 (operating pressure at the top of the tower) by a pitch delivery pump P103AB, wherein a part of the pitch is sent to granulation and a part of the pitch is sent to
Figure DEST_PATH_IMAGE043
) Further rectifying, and allowing the rectified light component gas to flow out of the top of the T101 tower (tower top operating temperature)
Figure 535455DEST_PATH_IMAGE044
) Condensed to the second tower coupling preheater E106
Figure 484956DEST_PATH_IMAGE045
Entering a second tower reflux tank V102, refluxing a part of the mixture to the second tower, and cooling a part of the mixture in a light oil cooler
Figure 246239DEST_PATH_IMAGE040
Then enters a light oil receiving tank V103 for temporary storage.
Two tower bottom (operating temperature)
Figure DEST_PATH_IMAGE046
) A circulating pump P105AB is arranged for forced circulation, the circulation returns to the tower bottom and the middle part of the tower again through a reboiler E108 and an evaporator E109, and the tower bottom is a qualified product
Figure 41019DEST_PATH_IMAGE047
A softening point pitch.
(2) Thermal polymerization
Qualified product at the bottom of the tower
Figure 204148DEST_PATH_IMAGE047
The pitch with softening point is fed in by a pitch delivery pump P106AB
Figure 324550DEST_PATH_IMAGE034
Carrying out thermal polymerization in a reaction kettle R101, and adding the raw materials into the reaction kettle in the thermal polymerization process
Figure DEST_PATH_IMAGE048
The liquid (G01 tank) is stirred and fully contacted with the asphalt until the pH value in the reaction kettle reaches
Figure 307550DEST_PATH_IMAGE049
(ii) a Thermal polymerization temperature maintenance of R101
Figure DEST_PATH_IMAGE050
Operating pressure of
Figure 658020DEST_PATH_IMAGE043
The residence time is
Figure 410076DEST_PATH_IMAGE051
(ii) a In the invention, the pH in the reaction kettle is measured by adopting a pre-installed pH sensor, and the brand is recommended to use
Figure DEST_PATH_IMAGE052
Temperature of use
Figure 435800DEST_PATH_IMAGE053
。
From
Figure 171675DEST_PATH_IMAGE034
The discharging material of the reaction kettle enters the reaction kettle through a delivery pump P109
Figure 839417DEST_PATH_IMAGE035
The reaction kettle R102 continues thermal polymerization, and asphalt quality is introduced within half an hour before thermal polymerization
Figure DEST_PATH_IMAGE054
Ammonium phosphate of (2)Benzene solution or benzene suspension (G02 tank), and heat polymerization is carried out for at least 1 hour after the benzene solution or benzene suspension is uniformly stirred in the heating process; temperature maintenance of R102
Figure 180400DEST_PATH_IMAGE055
At an operating pressure of
Figure 908184DEST_PATH_IMAGE043
The total residence time is
Figure DEST_PATH_IMAGE056
；
And condensing light component gas generated in the kettle through a kettle top condenser E111 and a kettle top aftercooler E112, collecting condensed light oil to V103, and periodically sending the collected light oil to a light oil storage tank in the tank area by the V103.
The reaction vessel R101 and the reaction vessel R102 do not undergo a pH adjustment step, and the pH is about 5 in the reaction process.
(3) Short path molecular distillation
The asphalt polymerized by the heat in the reaction kettle R102 is respectively sent to two sets of short-path molecular distillators E202A and E202B for processing the asphalt with high softening point. After entering the short-path molecular still, the asphalt is heated by the short-path molecular still to vaporize the light component, then the light component is led out and condensed, thus achieving the purpose that the light component and the heavy component (A)
Figure 396934DEST_PATH_IMAGE057
Pitch with softening point). The operation pressure of the short-path molecular evaporator is negative pressure, and the vacuum degree is
Figure 602788DEST_PATH_IMAGE043
. The jacket of the short-path molecular distillation device is heated by molten salt provided by a molten salt furnace, and the operation temperature is
Figure DEST_PATH_IMAGE058
。
The light component and the heavy component enter a light component receiving tank and a heavy component receiving tank which are matched with the light component and the heavy component. The medium in the light component receiving tank is low-softening-point asphalt which can be sent for granulation.
(4) Filtering and granulating
The recombination component is the coating material prepared by the invention, and the product is
Figure 63856DEST_PATH_IMAGE059
The medium in heavy component receiving tanks V202B and V202B is input into a material filter SXC01 through pumps P202A and P202B, the filtered asphalt enters a granulator for granulation (not shown in the figure), and the feeding temperature of the granulator is
Figure DEST_PATH_IMAGE060
。
After vertical bar magnet filter, again through horizontal bar magnet filter, recommend to use with high-efficient permanent magnet filter (shanghai chu can industry filtration system limited), bar magnet quantity: 7 size specifications:
Figure 165804DEST_PATH_IMAGE061
center distance
Figure DEST_PATH_IMAGE062
12000 Gauss magnetic bar, shot blasting on outer surface, and thickness of cylinder
Figure 79534DEST_PATH_IMAGE063
The device material is 304.
Comparative example 1
The comparative example differs from example 1 in that: in the first reaction kettle does not add
Figure DEST_PATH_IMAGE064
The rest steps are the same.
Comparative example 2
The comparative example differs from example 1 in that: no ammonium phosphate was added to the second reactor, and the rest of the procedure was the same.
Comparative example 3
The comparative example differs from example 1 in that: in the first reaction kettle does not add
Figure 557920DEST_PATH_IMAGE064
No ammonium phosphate was added to the second reactor, and the same procedure was followed.
Coating of
Figure 670232DEST_PATH_IMAGE065
Material, coating thickness
Figure DEST_PATH_IMAGE066
Constant current density
Figure 943081DEST_PATH_IMAGE067
First coulombic efficiency comparison: the invention
Figure DEST_PATH_IMAGE068
Comparison document (CN 113337304A)
Figure 406424DEST_PATH_IMAGE069
。
Figure DEST_PATH_IMAGE070
Figure 422921DEST_PATH_IMAGE071
Figure DEST_PATH_IMAGE072
Figure 858582DEST_PATH_IMAGE073
Figure DEST_PATH_IMAGE074
Although the embodiments of the present invention have been disclosed for illustrative purposes, those skilled in the art will appreciate that: various substitutions, changes and modifications are possible without departing from the spirit and scope of the invention and the appended claims, and therefore the scope of the invention is not limited to the embodiments disclosed.

Claims (2)

1. A production method of a graphite coating material is characterized by comprising the following steps: the method comprises the following steps:
(1) Rectification, namely obtaining the raw material ethylene tar through two-stage rectification
Figure DEST_PATH_IMAGE002
A softening point asphalt;
the rectification steps are as follows: ethylene tar passes through a two-tower coupling preheater and a one-tower coupling preheater, and the preheaters are preheated to the feeding temperature
Figure DEST_PATH_IMAGE004
Then enters a rectifying tower to be rectified, the rectified light component gas flows out from the top of the tower and is condensed to the bottom of the tower through a tower coupling preheater and a tower condenser
Figure DEST_PATH_IMAGE006
Entering a reflux tank of a tower, refluxing a part of the distillate to a tower of the rectification tower, and pumping a part of the distillate into a light oil cooler for cooling to
Figure DEST_PATH_IMAGE008
Then entering a light oil receiving tank for temporary storage;
a tower circulating pump is arranged at the bottom of the first rectifying tower for forced circulation, and the circulation returns to the bottom and the middle part of the first rectifying tower again through a tower reboiler and a tower evaporator; qualified product at the bottom of tower
Figure DEST_PATH_IMAGE010
The softened asphalt is sent to a first tower asphalt delivery pump for granulation, and sent to a second tower of a rectifying tower for further rectification, and the rectified light component gas flows out from the top of the second tower of the rectifying tower and is condensed to the second tower coupling preheater
Figure DEST_PATH_IMAGE012
Entering a reflux tank of the second tower, refluxing a part of the reflux liquid to the second tower of the rectifying tower, and cooling a part of the reflux liquid in a light oil cooler
Figure DEST_PATH_IMAGE014
Then entering a light oil receiving tank for temporary storage;
the bottom of the second tower of the rectifying tower is provided with a second tower circulating pump for forced circulation, the circulating pump returns to the bottom and the middle part of the second tower of the rectifying tower again after passing through a second tower reboiler and a second tower evaporator, and the bottom of the tower is a qualified product
Figure DEST_PATH_IMAGE016
A softening point asphalt;
(2) Heat polymerization: qualified product at the bottom of the tower
Figure DEST_PATH_IMAGE017
The pitch with softening point is sent into a first reaction kettle by a two-tower pitch delivery pump for thermal polymerization, and the heating is carried out in the reaction kettle in the process of thermal polymerization
Figure DEST_PATH_IMAGE019
Stirring for reaction until the pH value in the reaction kettle reaches
Figure DEST_PATH_IMAGE021
(ii) a Maintaining the thermal polymerization temperature of the first reaction vessel
Figure DEST_PATH_IMAGE023
Operating pressure of
Figure DEST_PATH_IMAGE025
The residence time is
Figure DEST_PATH_IMAGE027
；
Discharging from the first reaction kettle, feeding into the second reaction kettle via the delivery pump for continuous thermal polymerization, and introducing asphalt during the first half hour
Figure DEST_PATH_IMAGE029
The ammonium phosphate benzene solution or benzene suspension is heated and stirred evenly for at least 1 hour; temperature maintenance of the second reaction vessel
Figure DEST_PATH_IMAGE030
Operating pressure of
Figure 511501DEST_PATH_IMAGE025
Total residence time of
Figure DEST_PATH_IMAGE031
；
(3) Short path molecular distillation
Conveying the asphalt subjected to the thermal polymerization in the second reaction kettle to a short-distance molecular distiller for processing the asphalt with a high softening point; after entering the short-path molecular distiller, the asphalt is heated by the short-path molecular distiller to vaporize light components in the asphalt, and then the light components are led out and condensed, so that the light components and the heavy components are separated; obtaining the heavy fraction
Figure DEST_PATH_IMAGE033
A softening point asphalt; the operation pressure of the short-path molecular evaporator is negative pressure, and the vacuum degree is
Figure DEST_PATH_IMAGE034
；
(4) Filtering and granulating
Figure DEST_PATH_IMAGE035
The asphalt with softening point is input into the material through a pump for filtering, a magnetic filter is adopted for filtering, and the filtered asphalt enters a granulator for granulation.
2. The method for producing a graphite coating material according to claim 1, wherein: the jacket of the short-path molecular distillation device is heated by molten salt provided by a molten salt furnace.
CN202211070282.3A 2022-09-02 2022-09-02 Production method of graphite coating material Active CN115161054B (en)

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