CN114806620A - Pretreatment process for coal-based needle coke preparation raw material - Google Patents
Pretreatment process for coal-based needle coke preparation raw material Download PDFInfo
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- CN114806620A CN114806620A CN202111646681.5A CN202111646681A CN114806620A CN 114806620 A CN114806620 A CN 114806620A CN 202111646681 A CN202111646681 A CN 202111646681A CN 114806620 A CN114806620 A CN 114806620A
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- 239000002994 raw material Substances 0.000 title claims abstract description 52
- 239000011311 coal-based needle coke Substances 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title abstract description 17
- 238000002360 preparation method Methods 0.000 title description 3
- 239000002904 solvent Substances 0.000 claims abstract description 79
- 238000004062 sedimentation Methods 0.000 claims abstract description 73
- 238000004821 distillation Methods 0.000 claims abstract description 71
- 239000011294 coal tar pitch Substances 0.000 claims abstract description 49
- 238000004519 manufacturing process Methods 0.000 claims abstract description 38
- 239000011331 needle coke Substances 0.000 claims abstract description 32
- 238000002156 mixing Methods 0.000 claims abstract description 20
- 239000010426 asphalt Substances 0.000 claims description 31
- 239000000463 material Substances 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 12
- 238000004064 recycling Methods 0.000 claims description 11
- 239000011230 binding agent Substances 0.000 claims description 6
- 238000004939 coking Methods 0.000 claims description 6
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 abstract description 52
- 239000000126 substance Substances 0.000 abstract description 20
- 239000011295 pitch Substances 0.000 abstract description 13
- 239000013067 intermediate product Substances 0.000 abstract description 5
- 238000000926 separation method Methods 0.000 abstract description 3
- 238000000605 extraction Methods 0.000 abstract description 2
- 239000012046 mixed solvent Substances 0.000 abstract description 2
- 238000000638 solvent extraction Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 229910052717 sulfur Inorganic materials 0.000 description 4
- 239000011593 sulfur Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011300 coal pitch Substances 0.000 description 1
- 239000011280 coal tar Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000009628 steelmaking Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B57/00—Other carbonising or coking processes; Features of destructive distillation processes in general
- C10B57/08—Non-mechanical pretreatment of the charge, e.g. desulfurization
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B53/00—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form
-
- 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
-
- 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
- C10C3/005—Working-up pitch, asphalt, bitumen by mixing several fractions (also coaltar fractions with petroleum fractions)
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Civil Engineering (AREA)
- Structural Engineering (AREA)
- Working-Up Tar And Pitch (AREA)
- Coke Industry (AREA)
Abstract
The invention discloses a pretreatment process for preparing a raw material of coal-based needle coke, which comprises the following steps: (1) mixing the raw materials; (2) primary sedimentation; (3) secondary sedimentation; (4) heavy phase distillation; (5) distilling the light phase; (6) and (5) circulating the solvent. According to the invention, by adopting the principle of solvent extraction and sedimentation, two different solvents are mixed to form a mixed solvent, in order to improve the efficiency, extraction and sedimentation separation is carried out twice, then the separated heavy phase and light phase are separated by utilizing different densities, and finally the solvent is recovered by distillation. Through the innovative improvement of the process, the yield of the intermediate product refined pitch is improved, the quinoline insoluble substances can be effectively removed, the requirement on the content of the quinoline insoluble substances in the coal tar pitch is reduced, the raw material selection range is widened, and the aims of improving the yield of the needle coke and reducing the production cost of the needle coke are finally fulfilled.
Description
Technical Field
The invention relates to the technical field of coal chemical production, in particular to a pretreatment process for preparing a raw material of coal-based needle coke.
Background
The needle coke is a high-quality carbon material, is named after being crushed into a slender needle structure, has good orientation and strong electric and heat conducting properties, is a main raw material for manufacturing the ultrahigh-power graphite electrode, and the ultrahigh-power graphite electrode produced by using the needle coke has the advantages of low resistivity, large volume density, high mechanical strength, small thermal expansion coefficient, good thermal shock resistance and the like. The needle coke graphitized product is widely applied to the fields of electric furnace steel-making electrodes, nuclear reactor deceleration materials, rocket technology and the like.
Currently produced needle coke can be divided into two major types, namely oil-based needle coke and coal-based needle coke, according to different raw materials used in the process. Wherein, the oil-based needle coke is produced by taking catalytic oil slurry as a raw material, and the coal-based needle coke is produced by taking coal tar pitch and fractions thereof as raw materials.
For the production of coal-based needle coke, the following problems exist: firstly, most of the coal tar pitches have complex components, so that the coal tar pitch for producing coal-based needle coke products is always a product in short supply, and particularly the coal tar pitch for producing coal-based needle coke has higher environmental protection requirements in recent years, so that the coal tar pitch is increasingly in short supply, the price of the coal pitch is continuously increased, and the production cost of the needle coke is greatly increased. Secondly, in the production of the needle coke, the requirement on the content of quinoline insoluble substances in the raw material coal tar pitch is high, so that some coal pitches with high content of quinoline insoluble substances can not meet the requirement of raw materials for producing the needle coke. Therefore, in order to effectively utilize limited coal tar pitch resources, improve the yield of needle coke and produce high-quality needle coke, creative improvement is carried out on the production process of needle coke so as to improve the yield of needle coke, reduce the requirements of raw material coal tar pitch and finally reduce the production cost of needle coke, and the problems to be solved in the field are solved urgently.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a pretreatment process for preparing raw materials of coal-based needle coke, which is used for efficiently pretreating coal tar pitch serving as a raw material for producing the coal-based needle coke, and the yield of refined pitch serving as an intermediate product is improved on one hand through innovative improvement of the process; on the other hand, quinoline insoluble substances in the raw materials are efficiently removed, so that the requirement on the quinoline insoluble substances in the coal tar pitch is reduced, the selection range of the raw materials is widened, and the aims of improving the yield of the needle coke and reducing the production cost of the needle coke are finally fulfilled.
The invention provides a pretreatment process for preparing a raw material of coal-based needle coke, which comprises the following steps:
(1) mixing raw materials: according to the mass ratio (0.5-2): 1, mixing coal tar pitch and a solvent at 90-150 ℃ under normal pressure to obtain a mixed solution;
(2) primary sedimentation: before injecting materials, the mass ratio of solvent: coal tar pitch (0.1-0.5): 1, injecting a solvent into the bottom of a primary settling tank, adding the mixed solution obtained in the step (1) into the primary settling tank for primary settling treatment, wherein the temperature of primary settling is 90-150 ℃, the time of primary settling is 1-4 h, after the primary settling is finished, extracting the heavy component from the bottom of the primary settling tank, and extracting the light component from the top of the primary settling tank;
(3) secondary sedimentation: before injecting materials, the mass ratio of the solvent: coal tar pitch (0.1-0.5): 1, injecting a solvent into the bottom of a secondary sedimentation tank, adding the heavy component obtained in the step (2) into the secondary sedimentation tank for secondary sedimentation treatment, wherein the temperature of secondary sedimentation is 90-150 ℃, the time of secondary sedimentation is 1-4 h, after the secondary sedimentation is finished, the heavy component is obtained by being extracted from the bottom of the secondary sedimentation tank, and the light component is obtained by being extracted from the top of the secondary sedimentation tank;
(4) heavy phase distillation: adding the heavy component obtained in the step (2) into a heavy phase distillation tower for distillation treatment, extracting from the bottom of the heavy phase distillation tower to obtain binder asphalt, and extracting from the top of the heavy phase distillation tower to obtain a solvent;
(5) light phase distillation: adding the light components obtained in the step (2) and the step (3) into a light phase intermediate tank, conveying the light components to a heating furnace, heating the light phase intermediate tank to 200-260 ℃, conveying the light phase intermediate tank to a light phase distillation tower for distillation treatment, extracting the solvent from the top of the light phase distillation tower, and extracting the solvent from the bottom of the light phase distillation tower to obtain refined asphalt for needle coke coking production;
(6) solvent circulation: recycling the solvent obtained in the step (5) for mixing with the coal tar pitch in the step (1); and (4) recycling the solvent obtained in the step (4) and injecting the solvent into the bottoms of the primary settling tank and the secondary settling tank respectively in the step (2) and the step (3).
Preferably, the primary settling temperature in the step (2) is 100-120 ℃, and the primary settling time is 1.5-2.5 h.
Preferably, the secondary sedimentation temperature in the step (2) is 110-130 ℃, and the secondary sedimentation time is 2.5-3.5 h.
Preferably, in the step (4), the feeding temperature of the heavy phase distillation tower is 260-320 ℃, and the distillation treatment is carried out under micro negative pressure- (60-90) Pa.
Preferably, in the step (5), the feeding temperature of the light phase distillation tower is 210-250 ℃, and the distillation treatment is carried out under the micro negative pressure of- (60-90) Pa.
Preferably, the solvent used in the step (2) and the solvent used in the step (3): coal tar pitch 0.2: 1.
the reaction principle of the invention is as follows: the pretreatment process for preparing the raw materials of the coal-based needle coke utilizes the principle of solvent extraction and sedimentation, uses two different solvents to mix into a mixed solvent (one is dissolved and the other is separated), enriches quinoline insoluble substances in the raw material coal tar pitch to the bottom of a settling tank, separates out the quinoline insoluble substances as a heavy phase, and finally removes the quinoline insoluble substances in a liquid enrichment manner to finally obtain pure intermediate product refined pitch which accords with the production of the needle coke and is used for the production of the needle coke. Wherein: the primary sedimentation is primary extraction separation, the heavy phase also contains a part of effective refined asphalt, secondary sedimentation is carried out, further refined asphalt is extracted, and the sedimentation separation is carried out twice or more, so that on one hand, effective components in the soft asphalt can be further extracted to be used as the refined asphalt, the yield of the refined asphalt is improved, and on the other hand, the phenomenon that a large amount of quinoline insoluble substances at the bottom of the tank are accumulated to block pipelines and cause production accidents due to primary sedimentation is effectively avoided. Specifically, the method comprises the following steps: fully mixing the solvent and the raw material soft asphalt in the step (1); then, primarily extracting refined asphalt in the soft asphalt through the operation in the step (2), and primarily separating quinoline insoluble substances; in the step (3), the refined asphalt in the heavy phase is further extracted, so that the yield of the refined asphalt is improved, and the stable and safe operation of the device is ensured; and (3) recovering the solvent in the heavy phase in the step (4), recovering the solvent in the light phase in the step (5), and reusing the recovered solvent in the step (6), so that the production cost is reduced, and the device benefit is improved.
The invention has the beneficial effects that: the pretreatment process for preparing the raw materials of the coal-based needle coke carries out high-efficiency pretreatment on the coal tar pitch which is the production raw material of the coal-based needle coke, improves the yield of the refined pitch which is an intermediate product on one hand, can effectively remove quinoline insoluble substances on the other hand, reduces the requirement on the content of quinoline insoluble substances in the coal tar pitch, widens the selection range of the raw materials and finally achieves the aims of improving the yield of the needle coke and reducing the production cost of the needle coke. The method specifically comprises the following steps:
(1) the raw material range is widened: the high-efficiency pretreatment is carried out on the raw material coal tar pitch by a novel pretreatment process, so that the index requirement on quinoline insoluble substances in the raw material is reduced, the content of the quinoline insoluble substances in the raw material coal tar pitch is widened from the existing process requirement of being less than or equal to 3% to being less than or equal to 9%, the selection range of the raw material is widened, the raw material source is wider, and the raw material cost of an enterprise is reduced;
(2) the product yield is improved: the product yield of the pretreatment process is improved through the novel pretreatment process, so that the intermediate product refined asphalt is improved from 72 percent of the existing process to 82.5 percent, and the profit level of enterprises is improved.
Detailed Description
In order to make the technical solution of the present invention easier to understand, the technical solution of the present invention is now clearly and completely described by using the specific embodiments.
Example 1:
the pretreatment process for preparing the raw material of the coal-based needle coke comprises the following steps:
(1) mixing raw materials: according to the mass ratio of 0.5: 1, mixing coal tar pitch (0.6 percent of sulfur and 6.7 percent of quinoline insoluble) with a solvent at 90 ℃ and normal pressure to obtain a mixed solution;
(2) primary sedimentation: before injecting materials, the mass ratio of solvent: coal tar pitch 0.2: 1, injecting a solvent into the bottom of a primary settling tank, adding the mixed solution obtained in the step (1) into the primary settling tank for primary settling treatment, wherein the temperature of primary settling is 90 ℃, the primary settling time is 4 hours, and after the primary settling is finished, extracting the heavy component from the bottom of the primary settling tank and extracting the light component from the top of the primary settling tank;
(3) secondary sedimentation: before injecting materials, the mass ratio of the solvent: coal tar pitch 0.2: 1, injecting a solvent into the bottom of a secondary sedimentation tank, adding the heavy component obtained in the step (2) into the secondary sedimentation tank for secondary sedimentation treatment, wherein the temperature of secondary sedimentation is 120 ℃, the time of secondary sedimentation is 2 hours, after the secondary sedimentation is finished, the heavy component is obtained by being extracted from the bottom of the secondary sedimentation tank, and the light component is obtained by being extracted from the top of the secondary sedimentation tank;
(4) heavy phase distillation: adding the heavy component obtained in the step (2) into a heavy phase distillation tower, carrying out distillation treatment at the feeding temperature of 260 ℃ under the micro negative pressure of-60 Pa, extracting from the bottom of the heavy phase distillation tower to obtain binder asphalt, and extracting from the top of the heavy phase distillation tower to obtain a solvent;
(5) light phase distillation: adding the light components obtained in the step (2) and the step (3) into a light phase intermediate tank, conveying the light components to a heating furnace, heating the light components to 200 ℃, conveying the light components to a light phase distillation tower, carrying out distillation treatment at a feeding temperature of 210 ℃ under a micro negative pressure of-60 Pa, extracting the solvent from the top of the light phase distillation tower, and extracting the refined asphalt from the bottom of the light phase distillation tower, wherein the refined asphalt is used for needle coke coking production;
(6) solvent circulation: recycling the solvent obtained in the step (5) for mixing with the coal tar pitch in the step (1); and (4) recycling the solvent obtained in the step (4) and injecting the solvent into the bottoms of the primary settling tank and the secondary settling tank respectively in the step (2) and the step (3).
Example 2:
the pretreatment process for preparing the raw material of the coal-based needle coke comprises the following steps:
(1) mixing raw materials: according to the mass ratio of 1: 1, mixing coal tar pitch (0.6 percent of sulfur and 6.7 percent of quinoline insoluble) and a solvent at 110 ℃ and normal pressure to obtain a mixed solution;
(2) primary sedimentation: before injecting materials, the mass ratio of solvent: coal tar pitch 0.3: 1, injecting a solvent into the bottom of a primary settling tank, adding the mixed solution obtained in the step (1) into the primary settling tank for primary settling treatment, wherein the temperature of primary settling is 110 ℃, the time of primary settling is 3 hours, and after the primary settling is finished, extracting the heavy component from the bottom of the primary settling tank and extracting the light component from the top of the primary settling tank;
(3) secondary sedimentation: before injecting materials, the mass ratio of the solvent: coal tar pitch 0.3: 1, injecting a solvent into the bottom of a secondary sedimentation tank, adding the heavy component obtained in the step (2) into the secondary sedimentation tank for secondary sedimentation treatment, wherein the temperature of secondary sedimentation is 130 ℃, the time of secondary sedimentation is 1h, after the secondary sedimentation is finished, the heavy component is obtained by being extracted from the bottom of the secondary sedimentation tank, and the light component is obtained by being extracted from the top of the secondary sedimentation tank;
(4) heavy phase distillation: adding the heavy component obtained in the step (2) into a heavy phase distillation tower, carrying out distillation treatment at the feeding temperature of 280 ℃ under the micro negative pressure of-70 Pa, extracting from the bottom of the heavy phase distillation tower to obtain binder asphalt, and extracting from the top of the heavy phase distillation tower to obtain a solvent;
(5) light phase distillation: adding the light components obtained in the step (2) and the step (3) into a light phase intermediate tank, conveying the light components to a heating furnace, heating the light components to 215 ℃, conveying the light components to a light phase distillation tower, carrying out distillation treatment at a feeding temperature of 225 ℃ under a micro negative pressure of-70 Pa, extracting the solvent from the top of the light phase distillation tower, and extracting the refined asphalt from the bottom of the light phase distillation tower to obtain refined asphalt for the coking production of needle coke;
(6) solvent circulation: recycling the solvent obtained in the step (5) for mixing with the coal tar pitch in the step (1); and (5) circulating the solvent obtained in the step (4) and injecting the solvent into the bottoms of the primary settling tank and the secondary settling tank respectively in the step (2) and the step (3).
Example 3:
the pretreatment process for preparing the raw material of the coal-based needle coke comprises the following steps:
(1) mixing raw materials: according to the mass ratio of 1.5: 1, mixing coal tar pitch (0.58 percent of sulfur and 8.9 percent of quinoline insoluble) with a solvent at 130 ℃ and normal pressure to obtain a mixed solution;
(2) primary sedimentation: before injecting materials, the mass ratio of solvent: coal tar pitch 0.4: 1, injecting a solvent into the bottom of a primary settling tank, adding the mixed solution obtained in the step (1) into the primary settling tank for primary settling treatment, wherein the temperature of primary settling is 130 ℃, the time of primary settling is 2 hours, after the primary settling is finished, extracting the heavy component from the bottom of the primary settling tank, and extracting the light component from the top of the primary settling tank;
(3) secondary sedimentation: before injecting materials, the mass ratio of the solvent: coal tar pitch 0.4: 1, injecting a solvent into the bottom of a secondary sedimentation tank, adding the heavy component obtained in the step (2) into the secondary sedimentation tank for secondary sedimentation treatment, wherein the temperature of secondary sedimentation is 110 ℃, the secondary sedimentation time is 4 hours, after the secondary sedimentation is finished, the heavy component is obtained by being extracted from the bottom of the secondary sedimentation tank, and the light component is obtained by being extracted from the top of the secondary sedimentation tank;
(4) heavy phase distillation: adding the heavy component obtained in the step (2) into a heavy phase distillation tower, carrying out distillation treatment at the feeding temperature of 300 ℃ under the micro negative pressure of-80 Pa, extracting from the bottom of the heavy phase distillation tower to obtain binder asphalt, and extracting from the top of the heavy phase distillation tower to obtain a solvent;
(5) light phase distillation: adding the light components obtained in the step (2) and the step (3) into a light phase intermediate tank, conveying the light components to a heating furnace, heating the light components to 230 ℃, conveying the light components to a light phase distillation tower, carrying out distillation treatment at the feeding temperature of 240 ℃ under the micro negative pressure of-80 Pa, extracting the solvent from the top of the light phase distillation tower, and extracting the refined asphalt from the bottom of the light phase distillation tower, wherein the refined asphalt is used for the coking production of needle coke;
(6) solvent circulation: recycling the solvent obtained in the step (5) for mixing with the coal tar pitch in the step (1); and (4) recycling the solvent obtained in the step (4) and injecting the solvent into the bottoms of the primary settling tank and the secondary settling tank respectively in the step (2) and the step (3).
Example 4:
the pretreatment process for preparing the raw material of the coal-based needle coke comprises the following steps:
(1) mixing raw materials: according to the mass ratio of 2: 1, mixing coal tar pitch (0.45 percent of sulfur and 4.5 percent of quinoline insoluble) with a solvent at 150 ℃ and normal pressure to obtain a mixed solution;
(2) primary sedimentation: before injecting materials, the mass ratio of solvent: coal tar pitch 0.5: 1, injecting a solvent into the bottom of a primary settling tank, adding the mixed solution obtained in the step (1) into the primary settling tank for primary settling treatment, wherein the temperature of primary settling is 150 ℃, the primary settling time is 1h, and after the primary settling is finished, extracting the heavy component from the bottom of the primary settling tank and extracting the light component from the top of the primary settling tank;
(3) secondary sedimentation: before injecting materials, the mass ratio of the solvent: coal tar pitch 0.5: 1, injecting a solvent into the bottom of a secondary sedimentation tank, adding the heavy component obtained in the step (2) into the secondary sedimentation tank for secondary sedimentation treatment, wherein the temperature of secondary sedimentation is 100 ℃, the secondary sedimentation time is 3 hours, after the secondary sedimentation is finished, the heavy component is obtained by being extracted from the bottom of the secondary sedimentation tank, and the light component is obtained by being extracted from the top of the secondary sedimentation tank;
(4) heavy phase distillation: adding the heavy component obtained in the step (2) into a heavy phase distillation tower, carrying out distillation treatment at the feeding temperature of 320 ℃ under the micro negative pressure of-90 Pa, extracting from the bottom of the heavy phase distillation tower to obtain binder asphalt, and extracting from the top of the heavy phase distillation tower to obtain a solvent;
(5) light phase distillation: adding the light components obtained in the step (2) and the step (3) into a light phase intermediate tank, conveying the light components to a heating furnace, heating the light components to 240 ℃, conveying the light components to a light phase distillation tower, carrying out distillation treatment at the feeding temperature of 250 ℃ under the micro negative pressure of-90 Pa, extracting the solvent from the top of the light phase distillation tower, and extracting the refined asphalt from the bottom of the light phase distillation tower, wherein the refined asphalt is used for the coking production of needle coke;
(6) solvent circulation: recycling the solvent obtained in the step (5) for mixing with the coal tar pitch in the step (1); and (4) recycling the solvent obtained in the step (4) and injecting the solvent into the bottoms of the primary settling tank and the secondary settling tank respectively in the step (2) and the step (3).
Table 1: performance index of refined asphalt obtained in examples 1 to 4
Table 1 shows the performance indexes of the raw coal tar pitch and the refined pitch obtained by the preparation in examples 1 to 4, and the data in Table 1 are analyzed as follows:
first, as can be seen from the data in Table 1, the content of quinoline insoluble substances in the coal tar pitch used as the raw material in examples 1 to 4 was 2.97%, 6.7%, 8.9% and 4.5%, respectively, and the content of quinoline insoluble substances in the refined pitch obtained after pretreatment by the technique of the present invention was 0.01% or trace. That is, by the pretreatment process, the coal tar pitch with quinoline insoluble content as high as 9% can be used to prepare refined pitch with quinoline insoluble content of 0.01%, and the refined pitch meets the production requirements of needle coke and can be used as a high-quality raw material for producing needle coke. However, the coal tar pitch pretreated by the traditional process can be prepared into refined pitch meeting the production requirement of needle coke when the content of quinoline insoluble substances in the coal tar pitch is less than or equal to 3 percent. Therefore, after the technology is adopted, the quinoline insoluble substances in the coal tar pitch can be effectively removed through high-efficiency treatment of the coal tar pitch, and the high-quality refined pitch is prepared, so that the requirement on the content of the quinoline insoluble substances in the coal tar pitch which is a raw material for producing needle coke can be relaxed to 9%, and the selection range of the raw materials is widened.
Next, as can be seen from the data in table 1, the yields of refined pitches after pretreatment in examples 1 to 4 were 82.5%, 78.6%, 78.8% and 79.8%, respectively. And after the pretreatment by the traditional process, the yield of the refined asphalt is only 72 percent. Therefore, by the technology, the yield of the refined asphalt after pretreatment can be improved to 82.5 percent from 72 percent of the traditional pretreatment process, the yield of the refined asphalt can be improved by about 10 percent, and the effective utilization rate of the raw materials is greatly improved.
It should be noted that the embodiments described herein are only some embodiments of the present invention, and not all implementations of the present invention, and the embodiments are only examples, which are only used to provide a more intuitive and clear understanding of the present invention, and are not intended to limit the technical solutions of the present invention. All other embodiments, as well as other simple substitutions and various changes to the technical solutions of the present invention, which can be made by those skilled in the art without inventive work, are within the scope of the present invention without departing from the spirit of the present invention.
Claims (6)
1. A pretreatment process for preparing raw materials of coal-based needle coke is characterized by comprising the following steps:
(1) mixing raw materials: according to the mass ratio (0.5-2): 1, mixing coal tar pitch and a solvent at 90-150 ℃ under normal pressure to obtain a mixed solution;
(2) primary sedimentation: before injecting materials, the mass ratio of solvent: coal tar pitch (0.1-0.5): 1, injecting a solvent into the bottom of a primary settling tank, adding the mixed solution obtained in the step (1) into the primary settling tank for primary settling treatment, wherein the temperature of primary settling is 90-150 ℃, the time of primary settling is 1-4 h, after the primary settling is finished, extracting the heavy component from the bottom of the primary settling tank, and extracting the light component from the top of the primary settling tank;
(3) secondary sedimentation: before injecting materials, the mass ratio of the solvent: coal tar pitch (0.1-0.5): 1, injecting a solvent into the bottom of a secondary sedimentation tank, adding the heavy component obtained in the step (2) into the secondary sedimentation tank for secondary sedimentation treatment, wherein the temperature of secondary sedimentation is 90-150 ℃, the time of secondary sedimentation is 1-4 h, after the secondary sedimentation is finished, the heavy component is obtained by being extracted from the bottom of the secondary sedimentation tank, and the light component is obtained by being extracted from the top of the secondary sedimentation tank;
(4) heavy phase distillation: adding the heavy component obtained in the step (2) into a heavy phase distillation tower for distillation treatment, extracting from the bottom of the heavy phase distillation tower to obtain binder asphalt, and extracting from the top of the heavy phase distillation tower to obtain a solvent;
(5) light phase distillation: adding the light components obtained in the step (2) and the step (3) into a light phase intermediate tank, conveying the light components to a heating furnace, heating the light phase intermediate tank to 200-260 ℃, conveying the light phase intermediate tank to a light phase distillation tower for distillation treatment, extracting the solvent from the top of the light phase distillation tower, and extracting the solvent from the bottom of the light phase distillation tower to obtain refined asphalt for needle coke coking production;
(6) solvent circulation: recycling the solvent obtained in the step (5) for mixing with the coal tar pitch in the step (1); and (4) recycling the solvent obtained in the step (4) and injecting the solvent into the bottoms of the primary settling tank and the secondary settling tank respectively in the step (2) and the step (3).
2. The pretreatment process for preparing the raw material of the coal-based needle coke according to claim 1, wherein the primary settling temperature in the step (2) is 100 to 120 ℃, and the primary settling time is 1.5 to 2.5 hours.
3. The pretreatment process for preparing the raw material of the coal-based needle coke according to claim 1, wherein the secondary sedimentation temperature in the step (2) is 110 to 130 ℃, and the secondary sedimentation time is 2.5 to 3.5 hours.
4. The pretreatment process for preparing the raw material of the coal-based needle coke according to claim 1, wherein in the step (4), the heavy phase distillation tower is used for distillation treatment at the feeding temperature of 260-320 ℃ and under the micro negative pressure of- (60-90) Pa.
5. The pretreatment process for preparing the raw material of the coal-based needle coke according to claim 1, wherein the feeding temperature of the light phase distillation tower in the step (5) is 210-250 ℃, and the light phase distillation tower is subjected to distillation treatment under the micro negative pressure of- (60-90) Pa.
6. The pretreatment process for preparing a raw material of coal-based needle coke according to claim 1, wherein the solvent in the step (2) and the step (3): coal tar pitch 0.2: 1.
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