CN1217365A - Two-stage coking preparation method for needle-shaped coke of coal series - Google Patents

Two-stage coking preparation method for needle-shaped coke of coal series Download PDF

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CN1217365A
CN1217365A CN 98114371 CN98114371A CN1217365A CN 1217365 A CN1217365 A CN 1217365A CN 98114371 CN98114371 CN 98114371 CN 98114371 A CN98114371 A CN 98114371A CN 1217365 A CN1217365 A CN 1217365A
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coking
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oil
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CN1132895C (en
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戴惠筠
熊必能
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Acre Coking and Refractory Engineering Consulting Corp MCC
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Abstract

The production method of coal measure needle coke is characterized by that in addition to coal-tar, coal maltha, prepared coal maltha and coal-tar distillate oil as raw materials said invention also adds the by-product oil obtained by processing bitumen as a new raw material variety,and its production process includes the following steps: flashing, polycondensation and coking treatment to obtain the coal measure needle coke; and after flashing treatment, adding a fractionation treatment process, then making polycondensation treatment, and adopting bituminous circulating heating or external supplementary heating mode outside reactor still to provide heat quantity to make polycondensation of raw material, and the coking operation is implemented by two-stage method under the condition of constant temp. or variable temp. in delayed coking plant.

Description

The two-stage coking preparation method of coal-based needle coke
The invention belongs to the coking chemical technology, is the preparation method of a kind of advanced person's coal-based needle coke.
Japan adopts solvent method to produce coal-based needle coke, Chinese patent ZL86100675 and CN1172147A disclose two kinds of preparation methods that do not add the coal-based needle coke of solvent, though patent has plurality of advantages, but find that through practice weak point is arranged: (1) flash oil component boiling spread is very wide, brings difficulty to the polycondensation operation; (2) heat-supplying mode of polycondensation raw material makes heater outlet temperature too high, easily makes material in reactor slagging scorification occur, results in blockage; (3) coking operation adopts general " alternating temperature one-stage process ", often scurries accidents such as tower, tube coking.
In view of the problems referred to above that exist, the objective of the invention is to design a kind of raw material variety and enlarge, cost is low, product yield height, Functionality, quality and appealing design, technical process is reasonable, the preparation method of the coal-based needle coke of no coking and blocking phenomenon in the operation.
For achieving the above object, the technical measures taked of the present invention are two-stage coking preparation methods of a kind of coal-based needle coke of design.Four schemes are arranged, first scheme is that employing coal tar, coal viscid bitumen, preparation coal viscid bitumen or dead oil (as anthracene oil, a carbolineum, carbolineum cut etc.) are the flash distillation raw material, get flash oil polycondensation raw material through flash distillation, after polycondensation, get coking raw material, after coking handle coal-based needle coke, it is characterized in that: (1) also can adopt pitch processing to pay a produce oil is the flash distillation raw material; (2) carry out polycondensation again through separating treatment again after the flash distillation of flash distillation raw material; (3) the polycondensation raw material adopts the pitch circulation type of heating heating that Polycondensation Reactor and Esterification Reactor is come out, and perhaps adopts the outer heating jacket supplementary heating mode heat supply of reactor; (4) coking operation is in improved delayed coking unit, and coking raw material carries out carbonization and the operation of dry two-stage method under constant temperature or alternating temperature condition, stop into raw material in second section operation, and swap-in lightweight oil plant continues heat supply.Alternative plan is that employing coal tar, coal viscid bitumen, preparation coal viscid bitumen or dead oil (as anthracene oil, a carbolineum, carbolineum cut etc.) are the flash distillation raw material, get flash oil through flash distillation and directly make coking raw material, after coking handle coal-based needle coke, it is characterized in that: (1) also can adopt pitch processing to pay a produce oil is the flash distillation raw material; (2) coking operation is in improved delayed coking unit, and coking raw material carries out carbonization and the operation of dry two-stage method under constant temperature or alternating temperature condition, stop into raw material swap-in lightweight oil plant in second section operation, continues heat supply.The 3rd scheme is to adopt purified dead oil to make the polycondensation raw material, gets the polycondensation asphalt coking raw material through polycondensation, after coking handle coal-based needle coke, it is characterized in that: (1) also can adopt purified pitch processing to pay a produce oil is the polycondensation raw material; (2) the polycondensation raw material adopts the pitch circulation type of heating heating that Polycondensation Reactor and Esterification Reactor is come out, and perhaps adopts the outer heating jacket supplementary heating mode heat supply of reactor; (3) coking operation is in improved delayed coking unit, and coking raw material carries out carbonization and the operation of dry two-stage method under constant temperature or alternating temperature condition, in second section operation, stop into raw material, and swap-in lightweight oil plant continues heat supply.The 4th scheme is to adopt solvent method, distillation method, solvent-centrifuging, pure refined asphaltic bitumen that centrifuging etc. make or pure refining oil plant are made coking raw material, through coking handle coal-based needle coke, it is characterized in that coking operation is in improved delayed coking unit, coking raw material carries out carbonization and the operation of dry two-stage method under constant temperature or alternating temperature condition, stop into raw material in second section operation, swap-in lightweight oil plant continues heat supply.
The present invention is owing to take technique scheme, and the positively effect of generation is: (1) not only can make full use of raw material resources owing to enlarged raw material variety, can also improve product yield and optimize quality product.(2) scheme 1 adopts flash distillation to add fractionation technology, and flash oil is fractionated into two cut sections of light, heavy flash oil, and heavy flash oil is directly sent into coking operation, has simplified operating process.Light flash oil owing to only light flash oil component is arranged, narrows down its boiling spread as the polycondensation raw material, has improved the polycondensation service temperature, deepens the polycondensation degree, thereby has improved the yield and the quality of finished product.(8) because the polycondensation raw material adopts from the heating of the effusive pitch circulation of Polycondensation Reactor and Esterification Reactor type of heating, perhaps adopt the outer heating jacket supplementary heating mode heat supply of reactor, thereby reduced the temperature out of reactor, avoided material slagging scorification in the still and the fault that causes; Material is heated evenly in the still, and fully reaction has improved the polycondensation effect.(4) because coking operation adopts constant temperature or alternating temperature to carry out carbonization and the operation of dry two-stage method, make the raw material into coking tower all generate needle coke at low temperatures, the later stage is in high temperature, and high temperature gas flow carries out " drawing Jiao " and removes fugitive constituent, has improved quality product; Because the pitch coke that no high temperature generates down in the tower discharges of the coke without segmentation, has improved yield rate; Owing to do not retain liquid phase pitch in the boiler tube, so be difficult for coking and the tower accident is scurried in generation by easy coking pitch and Ta Nei.
Accompanying drawing is the process flow sheet of the two-stage coking preparation method of coal-based needle coke of the present invention.
Introduce technology contents of the present invention in detail below in conjunction with drawings and Examples.
Embodiment
As shown in drawings: with dead oil (carbolineum, anthracene oil, in, the narrow fraction of heavy boiling point composition, as , the firefly anthracene, anthracene, phenanthrene, carbazole, acenaphthene, biphenyl, naphthalene), coal tar, coal viscid bitumen, preparation coal viscid bitumen or pitch processing pay a produce oil (as the modified pitch flash oil, hard pitch flash oil, coking heavy oil, in, heavy aromatics component oil plant) be the flash distillation raw material; With pump 10 warp let-off process furnace 1, enter flashing tower 4, separation column 5 is passed through in flash distillation under the condition of 300~510 ℃ of vacuum tightness 0~98Kpa, temperature again, goes out heavy flash oil at the bottom of the tower, can directly make coking raw material; Overhead oil vapour gets light flash oil through condensate cooler 7, make the polycondensation raw material, perhaps the two all makes the polycondensation raw material, doing polycondensation respectively handles, the polycondensation raw material is sent into reactor 8 with pump 11 through process furnace 2, under 350~510 ℃ of temperature, pressure 0~3Mpa, 2~30 hours residence time condition, carry out polycondensation, can make softening temperature and be 0~80 ℃ polycondensation asphalt.The effusive polycondensation asphalt in 8 ends of reactor, a part be as coking raw material, most ofly carries out pitch circulation heating operation with new flash oil through pump 11.Smoked flash oil and polycondensation asphalt coking raw material are gone into 6 ends of separation column through pump 12, behind the oily vapour contact heat-exchanging in coking tower 9 tops, mix with turning oil.Mixing oil is through pump 13, and process furnace 3 is sent into coking tower 9, carries out the two-stage coking operation.During first section operation, process furnace 3 temperature outs are 400~500 ℃, under constant temperature or alternating temperature operational condition, carry out the low temperature liquid phase carbonizing treatment through coking tower 9 again, during second section operation, stop into raw material, and swap-in lightweight oil plant continues heat supply.High 5~40 ℃ when making process furnace 3 temperature outs than first section operation, under constant temperature or alternating temperature condition, in coking tower 9, carry out drying treatment, get coal-based needle coke at the bottom of the tower.Coking tower 9 tower top pressures are 0~1.5Mpa.Separation column 6 is 80~220 ℃ of tower top temperatures, pressure 0~1.3Mpa, and 150~450 ℃ of column bottom temperatures are operated under the condition of recycle ratio 0.5~3.Tower top side line gets coker light oil, and the bottom side line gets coking heavy oil, gets turning oil at the bottom of the tower and uses for systemic circulation.9 liang of tower alternate operations of coking tower, the cycle of the discharging of the coke is 24~48 hours, when first tower is filled coke and is transformed into second tower, still advances the lightweight oil plant and lowers the temperature, and then advance raw material to second tower, at this moment second working life begins.
The lightweight oil plant is not for containing the oil of coking composition, as various light ends oil or other lightweight oil of coker light oil, coking heavy oil, turning oil, polycondensation light oil, tar.
Because coking tower 9 inner foam layers rise, overhead oil vapour produces the material of carrying secretly and causing containing quinoline non-soluble impurity and brings in the system, so be provided with tower strainer 14 on the overhead oil steam pipe of coking tower 9 in order to prevent.
For regularly removing the cinder at 6 ends of separation column,, be provided with tower outer circulation oil strainer 15 in 6 ends of separation column to prolong the cycle of operation of system.
For avoiding reactor 8 bottom outlet pipe plug plugs, be provided with quenching apparatus 16 thereon, so that slow down the speed of response of material.
As being raw material, during by above-mentioned technical process and operational condition test, make coal-based needle coke and pair product-mid-temperature pitch or viscid bitumen in the scheme 1 with preparation coal viscid bitumen.Table 1,2,3 is listed preparation coal viscid bitumen material performance respectively, and mid-temperature pitch or viscid bitumen are paid quality product and coal-based needle coke quality product.
Table 1 preparation coal viscid bitumen material performance
??sp,℃ ??d,g/ml ??TI,% ?QI% ???V% ????S% ???A% Viscosity, E 50
?23.5 ??1.39 ???10 ??2 ??77.1 ????0.48 ????0.1 ????--
Table 2 mid-temperature pitch or viscid bitumen are paid quality product
Byproduct ?sp,℃ ?TI,% ??QI,% ???V% S% ???A% ??dg/ml
Mid-temperature pitch ????89 ???30 ????7 ???57.2 ?-- ???0.29 ???--
Viscid bitumen ????35 ???-- ????1.1 ???-- ?-- ???0.12 ???1.41
Table 3 coal-based needle coke quality product
Figure A9811437100071
The separating treatment of scheme 2 after reducing polycondensation program and flash distillation, other flow process is identical with scheme 1, i.e. the flash oil that gets after the flash distillation is directly as coking raw material.
Scheme 3 is except reducing flash distillation program and separating treatment thereafter, and other flow process is identical with scheme 1, and raw material must be pure oil, can be without flash distillation directly as the polycondensation raw material.
What scheme 4 and scheme 1,2,3 were different is to make coking raw material with other method---purified refined asphaltic bitumen material or purified refining oil plant, but coking operation is identical with scheme 1,2,3, is two-stage method.

Claims (13)

1, a kind of two-stage coking preparation method of coal-based needle coke, adopt coal tar, coal viscid bitumen, preparation coal viscid bitumen or dead oil, dead oil such as anthracene oil, a carbolineum, carbolineum cut etc. are the flash distillation raw material, get flash oil polycondensation raw material through flash distillation, after polycondensation, get the polycondensation asphalt coking raw material, after coking handle coal-based needle coke, it is characterized in that:
(1) also can adopt pitch processing to pay produce oil is the flash distillation raw material;
(2) carry out polycondensation again through separating treatment again after the flash distillation of flash distillation raw material;
(3) the polycondensation raw material adopts the pitch circulation type of heating heating that Polycondensation Reactor and Esterification Reactor is come out, and perhaps adopts the outer heating jacket supplementary heating heat supply of reactor;
(4) coking operation is in improved delayed coking unit, and coking raw material carries out carbonization and the operation of dry two-stage method under constant temperature or alternating temperature condition, stop into raw material in second section operation, and swap-in lightweight oil plant continues heat supply.
2, a kind of two-stage coking preparation method of coal-based needle coke, adopt coal tar, coal viscid bitumen, preparation coal viscid bitumen or dead oil, dead oil such as anthracene oil, a carbolineum, carbolineum cut etc. are the flash distillation raw material, get flash oil through flash distillation, directly as coking raw material, after coking handle coal-based needle coke, it is characterized in that:
(1) also can adopt pitch processing to pay produce oil is the flash distillation raw material;
(2) coking operation is in improved delayed coking unit, and coking raw material carries out carbonization and the operation of dry two-stage method under constant temperature or alternating temperature condition, stop into raw material in second section operation, and swap-in lightweight oil plant continues heat supply.
3, a kind of two-stage coking preparation method of coal-based needle coke, adopt purified dead oil such as anthracene oil, a carbolineum, carbolineum cut etc. to make the polycondensation raw material, after polycondensation the polycondensation asphalt coking raw material, after coking handle coal-based needle coke, it is characterized in that:
(1) also can adopt purified pitch processing to pay produce oil is the polycondensation raw material;
(2) the polycondensation raw material adopts the pitch circulation type of heating heating that Polycondensation Reactor and Esterification Reactor is come out, and perhaps adopts the outer heating jacket supplementary heating mode heat supply of reactor;
(3) coking operation is in improved delayed coking unit, and coking raw material carries out carbonization and the operation of dry two-stage method through constant temperature or alternating temperature, stops into raw material when second section operation, and swap-in lightweight oil plant continues heat supply.
4, a kind of two-stage coking preparation method of coal-based needle coke, the pure refined asphaltic bitumen or the pure refining oil plant that adopt solvent method, distillation method, solvent-centrifuging, centrifuging etc. to make are made coking raw material, through coking handle coal-based needle coke, it is characterized in that: coking operation is in improved delayed coking unit, coking raw material carries out carbonization and the operation of dry two-stage method under constant temperature or alternating temperature condition, stop into raw material in second section operation, swap-in lightweight oil plant continues heat supply.
5, the two-stage coking preparation method of a kind of coal-based needle coke according to claim 1 and 2 is characterized in that: the flash distillation of flash distillation raw material or separation condition are 300~510 ℃ of vacuum tightness 0~98Kpa, temperature.
6, the two-stage coking preparation method of a kind of coal-based needle coke according to claim 5 is characterized in that: the tripping device (5) that flashing tower (4) is provided with can adopt separation column or condenser.
7, according to the two-stage coking preparation method of claim 1 or 3 described a kind of coal-based needle cokes, it is characterized in that: the polycondensation condition of polycondensation raw material is 350~510 ℃ of temperature, pressure 0~3Mpa, and the residence time is 2~30 hours.
8, the two-stage coking preparation method of a kind of coal-based needle coke according to claim 7 is characterized in that: be provided with chilling facility (16) on reactor (8) bottom outlet pipe.
9, according to the two-stage coking preparation method of claim 1 or 2 or 3 described a kind of coal-based needle cokes, it is characterized in that: during dead oil can adopt, the narrow fraction of heavy boiling point composition, as , firefly anthracene, anthracene, phenanthrene, carbazole, acenaphthene, biphenyl, naphthalene; A produce oil is paid in pitch processing can adopt the modified pitch flash oil, the hard pitch flash oil, coking heavy oil, in, heavy aromatics component oil plant.
10, according to the two-stage coking preparation method of claim 1 or 2 or 3 or 4 described a kind of coal-based needle cokes, it is characterized in that: coking raw material is in first section operation, earlier through separation column (6), process furnace (3), heater outlet temperature is 400~500 ℃, under constant temperature or alternating temperature condition, carry out the low temperature liquid phase carbonizing treatment through coking tower (9) again; In second section operation, stop into raw material, swap-in lightweight oil plant continues heat supply, improves 5~40 ℃ when making process furnace (3) temperature out than first section operation, under constant temperature or alternating temperature condition, carries out drying treatment through coking tower (9) again; Coking tower (9) two tower alternate operations, the cycle of the discharging of the coke is 24~48 hours, when first tower is filled coke and is transformed into second tower, still advances the cooling of lightweight oil plant.
11, the two-stage coking preparation method of a kind of coal-based needle coke according to claim 10, it is characterized in that: it is 80~220 ℃ of separation column (6) tower top temperatures that coking raw material carries out the coking treatment condition, pressure 0~1.3Mpa, 150~450 ℃ of column bottom temperatures, recycle ratio 0.5~3, the tower top pressure 0~1.5Mpa of coking tower (9).
12, the two-stage coking preparation method of a kind of coal-based needle coke according to claim 10, it is characterized in that: the lightweight oil plant is not for containing the oil of coking composition, as various light ends oil or other lightweight wet goods of coker light oil, coking heavy oil, turning oil, polycondensation light oil, tar.
13, according to claim 10 the two-stage coking preparation method of fast a kind of coal-based needle coke, it is characterized in that: on the overhead oil steam pipe of coking tower (9), be provided with tower strainer (14), be provided with tower outer circulation oil strainer (15) in the bottom of separation column (6).
CN98114371A 1998-10-07 1998-10-07 Two-stage coking preparation method for needle-shaped coke of coal series Expired - Lifetime CN1132895C (en)

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1314779C (en) * 2005-07-19 2007-05-09 上海应用技术学院 Preparation method of needle coke
CN100462419C (en) * 2005-12-29 2009-02-18 中钢集团鞍山热能研究院 Tech. for preparing needle-shape coke using coal tar soft asphalt as raw material
CN102099438A (en) * 2008-07-31 2011-06-15 巴西石油公司 Process for production of bio-oil by coprocessing of biomass in a delayed coking unit
CN102295943A (en) * 2011-08-12 2011-12-28 中石油东北炼化工程有限公司葫芦岛设计院 Method for coking needle coke by large recycle ratio oil system
CN102634364A (en) * 2012-04-16 2012-08-15 中冶焦耐(大连)工程技术有限公司 Pretreatment technology of raw material asphalt used for producing needle-like coke
CN102634369A (en) * 2012-04-17 2012-08-15 焦云 High-temperature coal tar hydrogenation, post-delayed coking and methanol preparation by utilizing coke oven gas combined technology
CN103113908A (en) * 2013-01-30 2013-05-22 陕西煤业化工技术研究院有限责任公司 Coal-based needle coke preparation process
CN103614153A (en) * 2013-11-29 2014-03-05 神华集团有限责任公司 Preparation method of polycondensed asphalt, preparation method of needle coke and needle coke
CN108395904A (en) * 2018-04-04 2018-08-14 山西宏特煤化工有限公司 The pretreatment of raw material solvent extraction system and its method of needle coke industrialized production
CN110791315A (en) * 2019-11-15 2020-02-14 陕西师范大学 Method for preparing needle coke by using catalytic cracking slurry oil
CN111925814A (en) * 2020-07-22 2020-11-13 山东益大新材料股份有限公司 Delayed coking system and method for producing coal-series and oil-series needle coke in time-sharing manner
CN113048787A (en) * 2021-03-08 2021-06-29 中国神华煤制油化工有限公司 Heating furnace device for heating slurry, method for treating slurry and oil residue extraction system

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN86100675B (en) * 1986-01-20 1988-03-09 冶金工业部鞍山焦化耐火材料设计研究院 Method of producing coal based needle form coke
CN1063213C (en) * 1996-07-25 2001-03-14 沿海化工(鞍山)有限公司 Process for producing improved coal system needle coke

Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1314779C (en) * 2005-07-19 2007-05-09 上海应用技术学院 Preparation method of needle coke
CN100462419C (en) * 2005-12-29 2009-02-18 中钢集团鞍山热能研究院 Tech. for preparing needle-shape coke using coal tar soft asphalt as raw material
CN102099438A (en) * 2008-07-31 2011-06-15 巴西石油公司 Process for production of bio-oil by coprocessing of biomass in a delayed coking unit
CN102295943B (en) * 2011-08-12 2013-06-26 中石油东北炼化工程有限公司葫芦岛设计院 Method for coking needle coke by large recycle ratio oil system
CN102295943A (en) * 2011-08-12 2011-12-28 中石油东北炼化工程有限公司葫芦岛设计院 Method for coking needle coke by large recycle ratio oil system
CN102634364B (en) * 2012-04-16 2013-11-27 中冶焦耐(大连)工程技术有限公司 Pretreatment technology of raw material asphalt used for producing needle-like coke
CN102634364A (en) * 2012-04-16 2012-08-15 中冶焦耐(大连)工程技术有限公司 Pretreatment technology of raw material asphalt used for producing needle-like coke
CN102634369A (en) * 2012-04-17 2012-08-15 焦云 High-temperature coal tar hydrogenation, post-delayed coking and methanol preparation by utilizing coke oven gas combined technology
CN103113908A (en) * 2013-01-30 2013-05-22 陕西煤业化工技术研究院有限责任公司 Coal-based needle coke preparation process
CN103614153A (en) * 2013-11-29 2014-03-05 神华集团有限责任公司 Preparation method of polycondensed asphalt, preparation method of needle coke and 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
CN108395904A (en) * 2018-04-04 2018-08-14 山西宏特煤化工有限公司 The pretreatment of raw material solvent extraction system and its method of needle coke industrialized production
CN108395904B (en) * 2018-04-04 2023-11-03 山西宏特煤化工有限公司 Raw material pretreatment solvent extraction system and method for needle coke industrial production
CN110791315A (en) * 2019-11-15 2020-02-14 陕西师范大学 Method for preparing needle coke by using catalytic cracking slurry oil
CN111925814A (en) * 2020-07-22 2020-11-13 山东益大新材料股份有限公司 Delayed coking system and method for producing coal-series and oil-series needle coke in time-sharing manner
CN113048787A (en) * 2021-03-08 2021-06-29 中国神华煤制油化工有限公司 Heating furnace device for heating slurry, method for treating slurry and oil residue extraction system
CN113048787B (en) * 2021-03-08 2022-10-18 中国神华煤制油化工有限公司 Heating furnace device for heating slurry, method for treating slurry and oil residue extraction system

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