CN1063213C - Process for producing improved coal system needle coke - Google Patents
Process for producing improved coal system needle coke Download PDFInfo
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- CN1063213C CN1063213C CN96115485A CN96115485A CN1063213C CN 1063213 C CN1063213 C CN 1063213C CN 96115485 A CN96115485 A CN 96115485A CN 96115485 A CN96115485 A CN 96115485A CN 1063213 C CN1063213 C CN 1063213C
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- coking
- needle coke
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Abstract
The present invention discloses a production process of improved coal measure needlelike coke, which is characterized in that anthracene oil, dianthracene oil or an anthracene oil distillation fraction in which a quinolinic insoluble substance and asphalt are removed is adopted as a raw material condensed and polymerized at the temperature of 350 to 490DEG C at the pressure of 0.5 to 3.0MPa, a condensed polymer together with circulating medium oil are conveyed into a heating furnace, operated at the variable temperature of 390 to 530DEG C and then operated in a coking tower at variable pressure maintained between 0MPa and 0.8MPa, the retention time is from 24 to 48 hours, and oil vapor starts to be blown into the coking tower in the last 1 to 10 hours to obtain the needlelike coke. The process has the advantages of no coking phenomenon and no blocking phenomenon. The weight yield can reach 40%.
Description
The present invention relates to the production technique of improved coal-based needle coke.
Chinese patent CN8610067.5 discloses a kind of novel preparation method of coal-based needle coke, system is a raw material with coal tar, coal viscid bitumen or preparation pitch, do not add solvent, only heat and the vacuum flashing processing, extract the mid-boiling point cut and get pure oil plant, must be suitable for the polycondensation asphalt of mesophase ball bulk-growth again through thermal polycondensation, and then in improved delayed coking unit, carry out coking handle coal-based needle coke.Yet this method has open defect: one, and coking and blocking appears in polycondensation easily, and cause suitability for industrialized production to be difficult to carry out.Its two, the needle coke product yield is on the low side (weight yield only reaches 20.5%), economical give birth to poor.
The objective of the invention is provides a kind of and do not produce coking and blocking in polycondensation by changing raw material and production technique thereof, and the production technique of the obvious improved coal-based needle coke that improves of yield.
Above-mentioned purpose of the present invention adopts following technical scheme to be achieved:
Technology of the present invention is:
To remove quinoline insolubles and bituminous one carbolineum, anthracene oil or carbolineum fraction are raw material, in temperature 350-490 ℃, polycondensation under the pressure 0.5-3.0MPa condition, the residence time is 6-26 hour.Oil (recycle ratio is 0.6-3.0) is sent into process furnace in the circulation of being allocated into together with separation column bottom by the effusive polycondensate of batch condensation polymerization reactor, in heater outlet temperature is 390-530 ℃ of alternating temperature operation, enter coking tower then, polycondensate is transformation operation under the 0-0.8MPa condition at tower top pressure, further polycondensation, generate mesophasespherule, growth is melted also then, is 24-48 hour at dwell time in the tower, in coking tower, blow oily vapour beginning in last 1-10 hour, get needle coke.
Because the present invention has adopted technique scheme, thereby has thoroughly solved the polycondensation coking and blocking problem, makes suitability for industrialized production be able to smooth implementation.And increased substantially the product weight yield, and can reach 40%, have favorable economic benefit.
Fig. 1 is a process flow sheet of the present invention.
Fig. 2 is a coking twenty four hours transformation graphic representation.
Fig. 3 is 40 hours transformation graphic representations of coking.
Followingly the present invention is commented with reference to Fig. 1-3 and embodiment and embodiment:
The concrete technology of the present invention is:
One carbolineum, anthracene oil or its mixture (having isolated pitch) or carbolineum fraction enter the 4# reactor with the heavy oil of separation column bottom together after the hot stove heating of 1# power, at temperature 350-490 ℃, polycondensation under the pressure 0.5-3.0MPa condition, the residence time be 6-26 hour (as containing impurity such as quinoline insolubles in the mixture, need to enter flashing tower 3# through the hot stove of 1# power, vacuum tightness is 13.3-92KPa in the tower, the be removed pure raw material (polycondensation heavy oil) of quinoline insolubles of its top, the bottom obtains byproduct one flash distillation heavy oil.The pure oil plant that comes out in the flashing tower top removes the hot stove of 1# power after condenser 11# cooling.
Polycondensation heavy oil is come out to send into the hot stove of 2# power together with oil in the separation column effusive circulation in bottom (Control Circulation is than being 0.5-3.0) by the 4# reactor bottom, heater outlet temperature is 390-530 ℃, the alternating temperature operation, enter coking tower 6# then, polycondensation heavy oil is further polycondensation under the 0-0.8MPa spare at tower top pressure, carries out thermal conversion reaction, generates mesophasespherule, grow then, melt also, get needle coke at last.At dwell time in the tower is 24-48/ hour.When last 1-10, begin at the bottom of tower, in coking tower, to blow oily vapour.Stop into raw material, thereby reduce the green coke fugitive constituent, promote burnt maturation, after a tower is filled coke, switch to another tower, two tower alternate operations, coking tower top oil vapour enters separation column 5# bottom.
The separation column head temperature is 100-220 ℃, and bottom temp is 210-460 ℃, and pressure is 0-0.7MPa, and overhead oil vapour gets light oil (can be used as and blow oil gas) after condenser 12# condensation, and heavy oil blows oily vapour as coking.
Described recycle ratio is the weight ratio of oil in polycondensation oil and the circulation.
Described oily vapour controlling index be the 3-7 ton/hour, the part by weight of itself and polycondensation heavy oil is: 0.5: 1.5.
Described oily vapour can be coking heavy oil, coker light oil or coking washing oil etc.
Present embodiment selects the quality index of raw material to be:
Mix the carbolineum fraction:
Viscosity (E100) 1.15-1.35 initial boiling point 〉=230 ℃
Quantity of distillate≤40% before 360 ℃ of density (e100) 1.09-1.15
One carbolineum
Viscosity (d20 ℃) 1.05-1.1
Initial boiling point: 〉=230 ℃
Quantity of distillate before 300 ℃ :≤15%
Anthracene oil
Viscosity: (d.20 ℃): 1.2-1.5
Initial boiling point: 〉=230 ℃
360 ℃ of quantity of distillate :≤40%
Above-mentioned raw materials all selects 420 ℃ to be the temperature point of contact, to isolate pitch impurity.
Control polycondensation heavy oil quality index is:
Viscosity (E100) 1.5-3.5
Quinoline insolubles Qi%≤0.2
Below provide the embodiment that selects according to embodiment of the present invention, see Table 1
Described transformation condition can be selected:
In 0-5 hour, keep constant voltage 0.05MPa, rate of pressure rise is 0.01MPa/h between 5-16 hour, rate of pressure rise is 0.04MPa/h between 16-32 hour, in 0.8Mpa constant voltage 〉=6 hour, perhaps, kept constant voltage 0.05MPa in 0-5 hour, rate of pressure rise is 0.05MPa/h between 5-18 hour, is constant voltage between 18-24 hour.
Claims (3)
1, the production technique of improved coal-based needle coke, it is characterized in that: to remove quinoline insolubles and to isolate a carbolineum of pitch composition, anthracene oil or carbolineum fraction are raw material, get the polycondensation heavy oil of higher carbon residue through thermal polycondensation, carrying out coking then in improved delayed coking unit handles, and adopt and to blow oily vapour technology and get coal-based needle coke, specifically tie up to temperature 350-490 ℃, pressure 0.5-3.0Pa, the residence time is generation polycondensation in 6-26 hour and cracking, oil is to enter process furnace under the 0.6-3.0 condition by anharmonic ratio in the circulation of being allocated into together with separation column bottom by the effusive polycondensation heavy oil of polycondensation reactor, in heater outlet temperature is 390-530 ℃ of alternating temperature operation, enter coking tower then, tightening heavy oil is transformation operation under the 0-0.8Mpa condition at tower top pressure, the residence time is 24-48 hour, in coking tower, blow oily vapour beginning in last 1-10 hour, get needle coke.
2, technology according to claim 1, it is characterized in that: described transformation operational condition is: kept constant voltage 0.05MPa in 0-5 hour, rate of pressure rise is 0.01MPa/h between 5-16 hour, and rate of pressure rise is 0.04MPa/h between 16-32 hour, in 0.8MPa constant voltage 〉=6 hour.
3, technology according to claim 1 is characterized in that: described transformation operational condition is: kept constant voltage 0.05MPa in 0-5 hour, rate of pressure rise is 0.05MPa/h between 5-18 hour, is constant voltage between 18-24 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96115485A CN1063213C (en) | 1996-07-25 | 1996-07-25 | Process for producing improved coal system needle coke |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96115485A CN1063213C (en) | 1996-07-25 | 1996-07-25 | Process for producing improved coal system needle coke |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1172147A CN1172147A (en) | 1998-02-04 |
| CN1063213C true CN1063213C (en) | 2001-03-14 |
Family
ID=5122731
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN96115485A Expired - Fee Related CN1063213C (en) | 1996-07-25 | 1996-07-25 | Process for producing improved coal system needle coke |
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| Country | Link |
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| CN (1) | CN1063213C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1323131C (en) * | 2004-03-31 | 2007-06-27 | 中国石油化工股份有限公司 | Delayed coking method for increasing coke strength |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1132895C (en) * | 1998-10-07 | 2003-12-31 | 中国冶金建设集团鞍山焦化耐火材料设计研究总院 | Two-stage coking preparation method for needle-shaped coke of coal series |
| CN1118537C (en) * | 2000-09-09 | 2003-08-20 | 沿海化工(鞍山)有限公司 | Process for preparing needle coke |
| CN1314779C (en) * | 2005-07-19 | 2007-05-09 | 上海应用技术学院 | Preparation method of needle coke |
| CN103113908B (en) * | 2013-01-30 | 2014-07-02 | 陕西煤业化工技术研究院有限责任公司 | Coal-based needle coke preparation process |
| CN104130792A (en) * | 2013-05-02 | 2014-11-05 | 山东宝舜化工科技有限公司 | Asphalt tubular furnace and technology for modifying asphalt by employing the asphalt tubular furnace |
| CN104560104B (en) * | 2013-10-23 | 2016-08-17 | 中国石油化工股份有限公司 | A kind of method producing needle coke |
| CN103614153B (en) * | 2013-11-29 | 2015-06-24 | 神华集团有限责任公司 | Preparation method of polycondensed asphalt, preparation method of needle coke and needle coke |
| CN114836230B (en) * | 2021-02-02 | 2023-04-25 | 圣德光科技发展(北京)有限公司 | Preparation method of binder and impregnant |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2728605A1 (en) * | 1977-06-24 | 1979-01-18 | Nittetsu Chem Ind Co | Needle coke from coal tar pitch - treated to ppte. quinoline-insolubles by addn. of aromatic and aliphatic solvents |
| US4547284A (en) * | 1982-02-16 | 1985-10-15 | Lummus Crest, Inc. | Coke production |
-
1996
- 1996-07-25 CN CN96115485A patent/CN1063213C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2728605A1 (en) * | 1977-06-24 | 1979-01-18 | Nittetsu Chem Ind Co | Needle coke from coal tar pitch - treated to ppte. quinoline-insolubles by addn. of aromatic and aliphatic solvents |
| US4547284A (en) * | 1982-02-16 | 1985-10-15 | Lummus Crest, Inc. | Coke production |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1323131C (en) * | 2004-03-31 | 2007-06-27 | 中国石油化工股份有限公司 | Delayed coking method for increasing coke strength |
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| Publication number | Publication date |
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| CN1172147A (en) | 1998-02-04 |
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