CN101126027A - Method for preparing coal series needle coke - Google Patents

Method for preparing coal series needle coke Download PDF

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Publication number
CN101126027A
CN101126027A CNA2006100474681A CN200610047468A CN101126027A CN 101126027 A CN101126027 A CN 101126027A CN A2006100474681 A CNA2006100474681 A CN A2006100474681A CN 200610047468 A CN200610047468 A CN 200610047468A CN 101126027 A CN101126027 A CN 101126027A
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oil
raw material
coking
flash
tower
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CNA2006100474681A
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Chinese (zh)
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戴惠筠
戴华
许国
何云
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Abstract

The invention relates to a coal-based needle coke and a production method thereof. Coal-series soft-asphalt or prepared soft-asphalt is taken as raw material. The process method the coal-based needle coke is divided into the steps: flash evaporation, condensation pretreatment, carbonization, drying, oil-gas purification and coking treatment. The invention is characterized in that heavy, medium and light three kinds of flash oil are obtained through condensation by step in flash evaporation process, then the three kinds of flash oil are treated respectively; a reaction vessel is provided with material feeding distribution pipe group and axially stirrer in the condensation treatment process, and the bottom of the reaction vessel takes a shape of taper; the purifying oil in the coking process is used in cycling; nitrogen substitutes for water steam poured in together with coking material; petroleum components is added into the flash or the condensation or the coking material to do co-carbonization; the byproducts of high-temperature asphalt, impregnant, adhesive, carbon black can be obtained after the pretreatment process. The technical measures of the invention have advanced technique, can make first-grade coal-based needle coke product, saves equipment blocking and can be smoothly operated.

Description

A kind of preparation method of coal series needle coke
Technical field
The present invention relates to the coking chemical technology, especially a kind of coal series needle coke preparation method.
Background technology
The preparation method of coal-based needle coke has multiple, but is good with distillation method.Existing ZL86100675.5, ZL98114371.7, CN1769373 and CN1304974A patented technology, progressively take innovative approach, make the preparation technique of coal-based needle coke more and more perfect, prepared fine fodder QI value is~0%, but because the fine fodder that is produced is the full cut of flash oil or only divides two sections, the very wide or broad of the molecular weight ranges of its composition is not easy to obtain the needle coke of first grade.Polycondensation charging inequality.Influence spherular growth with the concurrently injected water vapour of coking raw material.Pyrogenic reaction speed is slow.In order further to improve the quality of coal-based needle coke, should take new technical measures, develop new product.
Summary of the invention
The problems referred to above in view of existing the objective of the invention is to develop a kind of first grade coal-based needle coke preparation method that obtains.
In order to realize purpose of the present invention, the technical measures of taking are a kind of coal series needle coke preparation methods of design, adopt coal measures viscid bitumen or preparation viscid bitumen as the flash distillation raw material, make flash oil through the flash distillation pre-treatment, its QI value is~0%, the weight molecule flash oil is directly made coking raw material, the part flash oil is made the polycondensation raw material and adds petroleum component to carry out polycondensation, remake coking raw material through over-quenching, the advanced coking raw material of coking operation advances lightweight oil again, charging variable operation makes needle coke after finishing charing and solid phase drying process, and coking oil vapour carries out purifying treatment; It is characterized in that: 1) eject the flash oil that comes and carry out fractional condensation by three partial condensers 3,4,5 outside the tower from flashing tower 2, install on flashing tower 2 top perhaps that two partial condensers carry out fractionation and fractional condensation processing fractionation plant and tower outside, obtain heavy flash oil a, middle flash oil b and light flash oil c respectively, heavy flash oil a can directly send into coking tower 8 and make coking raw material, middle flash oil b generates polycondensation asphalt d and remakes coking raw material after polycondensation, light flash oil c remakes coking raw material or middle flash oil b and light flash oil c in case of necessity after degree of depth polycondensation can make other raw material; 2) being provided with the pan feeding distribution piping group of inserting liquid level in the still on the top of batch condensation polymerization reactor 6, being provided with axial agitator in the still, is taper at the bottom of the still; 3) replace with nitrogen h with the concurrently injected water vapour of the coking raw material that enters tubular oven 9, its amount is the 4-6% of raw material weight; 4) the self-cleaning oil g of coking oil vapour n 1Adopt mink cell focus, recycle, and outside the part removal system, with clean-up stage top backflow f 2Replenish; 5) petroleum component m can add respectively in flash distillation raw material or polycondensation raw material or the coking raw material according to different boiling, carries out common charing, and its amount is the 5-60% of raw material weight.
Oil also can make the hard pitch byproduct at the bottom of described flashing tower 2 towers except can producing modified pitch, mid-temperature pitch, oil fuel, and the cat head fine fodder can be produced high-quality soaker and binding agent or make the carbon black feed stock byproduct.
Advantage of the present invention is: the flash distillation pre-treatment can make the molecular weight ranges of flash oil narrow down, and can improve the needle coke quality; Reactor is established pan feeding distribution piping group and axial agitator, is taper at the bottom of the tower, and charging is mixed, sufficient reacting, and discharging is smooth; Replace the destruction that to avoid water vapour that microsphere is grown up with nitrogen with the concurrently injected water vapour of coking raw material; The self-cleaning oil of coking oil vapour recycles, fully heat exchange and make operation reasonable; Petroleum component adds in flash distillation raw material or polycondensation raw material or the coking raw material, carries out common charing, and the accelerated reaction process can be improved the needle coke quality.
Description of drawings
Accompanying drawing is a kind of process flow sheet of coal series needle coke preparation method.
In the accompanying drawing, 1,7,9 tubular ovens, 3,4,5 partial condensers, 2 flashing towers, 6 reactors, 8 coking towers, 10 separation columns, 11,12 interchanger.
As shown in drawings, adopt coal measures viscid bitumen or preparation viscid bitumen as the flash distillation raw material, through the flash distillation pre-treatment make heavy, in, light three kinds of flash oil a, b, c, handle respectively, the molecular weight ranges of every kind of flash oil is narrowed down, can improve the quality of needle coke.Being provided with the pan feeding distribution piping group of inserting liquid level in the still on the top of reactor 6, being provided with axial agitator in the still, is taper at the bottom of the still; Charging is mixed, sufficient reacting, discharging is smooth, avoids equipment to stop up.Replace the destruction that to avoid water vapour that microsphere is grown up with nitrogen h with the concurrently injected water vapour of the coking raw material that enters tubular oven 9.The self-cleaning oil g of coking oil vapour n 1Recycle, fully heat exchange and make operation rationally.Petroleum component m can add respectively in flash distillation raw material or polycondensation raw material or the coking raw material according to different boiling, carries out common charing, and accelerated reaction speed can be improved the needle coke quality.
Embodiment
Introduce the detailed content and the operating process of a kind of coal series needle coke preparation method of the present invention in conjunction with the accompanying drawings and embodiments: as shown in drawings, with the coal measures viscid bitumen is raw material, enter in the flashing tower 2 through tubular oven 1 (the pipe temperature out is 400-480 ℃), liquid phase is hard pitch q (temperature is 350-390 ℃) at the bottom of the tower, and the oily vapour k that cat head comes out (temperature is 380-450 ℃) enters partial condenser 3,4,5 must weigh flash oil a, middle flash oil b and light flash oil c.Heavy flash oil a can directly send into coking tower 8 and make coking raw material; Light flash oil c can make other raw material; Middle flash oil b makes the polycondensation raw material, flow to earlier in the circulation polycondensation asphalt p pipe before the tubular oven 7, entering reactor 6 through tubular oven 7 (temperature out is 430-460 ℃) carries out polycondensation together with circulation polycondensation asphalt p, service temperature in the reactor 6 is 420-450 ℃, working pressure is 1.0-1.5Mpa, reaction times is 6-15 hour, obtain qualified polycondensation asphalt d (softening temperature 10-35 ℃), go out in reactor 6 underflows together with circulation polycondensation asphalt p again, after polycondensation asphalt finished product d told, flash oil b entered tubular oven 7 cyclical operations during circulation polycondensation asphalt p added again, and the polycondensation asphalt finished product d that tells delivers to coking process and makes coking raw material behind chilling.Heavy flash oil a and polycondensation asphalt finished product d together enter coking tower 8 behind the adding petroleum component m, in the fill process, at the heating tube high temperature position nitrogen injection h of tubular oven 9 as coking raw material before tubular oven 9.In cycle, begin advanced coking raw material at a tower, coking tower 8 temperature ins are 470-500 ℃, constant temperature method in the time of last 8-10 hour, advances lightweight oil e to charging, carries out La Jiao and drying, first then constant temperature 4-6 hour, heater outlet temperature is improved 5-40 ℃ again, tower top pressure is 0-1.5Mpa; Coking tower 8 overhead oil vapour n enter at the bottom of separation column 10 towers, at this and self-cleaning oil g 1Convective heat exchange and flushing, the overhead oil vapour n after cleaning is raised to plate again, squeezes into clean-up stage top backflow f 2Carry out fractionation, do to purify for the second time, overhead oil vapour n rises to the above separation column section of blind column plate then, continues to handle routinely, and tower top temperature is 100-250 ℃, and pressure is 0-1.4Mpa, self-cleaning oil g 1Be mink cell focus, recycle, and part self-cleaning oil g 2Outside the removal system, with clean-up stage top backflow f 2Replenish; Coking raw material enters interchanger 11, with self-cleaning oil g 1Enter interchanger 12 after the heat exchange again, with thermal cycling heavy oil f 1Heat exchange adds thermal cycling heavy oil f then 1Enter coking tower 8 through tubular oven 9 and carry out coking operation.Coking cycle is 24-48 hour, and recycle ratio is 0.5-1.5, two tower alternate operations.

Claims (2)

1. the preparation method of a coal series needle coke, adopt coal measures viscid bitumen or preparation viscid bitumen as the flash distillation raw material, make flash oil through the flash distillation pre-treatment, its QI value is~0%, and the weight molecule flash oil is directly made coking raw material, the part flash oil is made the polycondensation raw material and adds petroleum component to carry out polycondensation, remake coking raw material through over-quenching, the advanced coking raw material of coking operation advances lightweight oil again, the operation of charging variable, make needle coke after finishing charing and solid phase drying process, coking oil vapour carries out purifying treatment; It is characterized in that:
1) ejects the flash oil that comes from flashing tower (2) and pass through three partial condensers (3) outside the tower, (4), (5) carry out fractional condensation, install on flashing tower (2) top perhaps that two partial condensers carry out fractionation and fractional condensation processing fractionation plant and tower outside, obtain heavy flash oil a respectively, middle flash oil b and light flash oil c, heavy flash oil a can directly send into coking tower (8) and make coking raw material, middle flash oil b generates polycondensation asphalt d and remakes coking raw material after polycondensation, light flash oil c remakes coking raw material in case of necessity after degree of depth polycondensation, perhaps middle flash oil b and light flash oil c can make other raw material;
2) being provided with the pan feeding distribution piping group of inserting liquid level in the still on the top of batch condensation polymerization reactor (6), being provided with axial agitator in the still, is taper at the bottom of the still;
3) replace with nitrogen h with the concurrently injected water vapour of the coking raw material that enters coking tower (8), its amount is the 4-6% of raw material weight;
4) the self-cleaning oil g of coking oil vapour n 1Adopt mink cell focus, recycle, and outside the part removal system, with clean-up stage top backflow f 2Replenish;
5) petroleum component m can add respectively in flash distillation raw material or polycondensation raw material or the coking raw material according to different boiling, carries out common charing, and its amount is the 5-60% of raw material weight.
2. the preparation method of a kind of coal series needle coke according to claim 1, oil also can make the hard pitch byproduct at the bottom of it is characterized in that flashing tower (2) tower except can producing modified pitch, mid-temperature pitch, oil fuel, and the cat head fine fodder can be produced high-quality soaker and binding agent or make the carbon black feed stock byproduct.
CNA2006100474681A 2006-08-17 2006-08-17 Method for preparing coal series needle coke Pending CN101126027A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101580242B (en) * 2009-06-15 2011-03-16 太原理工大学 Method for preparing needle coke by coal-tar asphalt
CN102051191A (en) * 2009-11-03 2011-05-11 上海宝钢化工有限公司 Production method and system of coal-based needle coke
CN102329526A (en) * 2011-07-25 2012-01-25 万西赣 Production process and equipment of carbon black for rubber produced by using maltha
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
CN104694146A (en) * 2015-04-09 2015-06-10 河南开炭新材料有限公司 Flashing and pressure holding combined retention tower electric tracing heating temperature holding modified pitch production technology

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101580242B (en) * 2009-06-15 2011-03-16 太原理工大学 Method for preparing needle coke by coal-tar asphalt
CN102051191A (en) * 2009-11-03 2011-05-11 上海宝钢化工有限公司 Production method and system of coal-based needle coke
CN102051191B (en) * 2009-11-03 2013-07-24 上海宝钢化工有限公司 Production method and system of coal-based needle coke
CN102329526A (en) * 2011-07-25 2012-01-25 万西赣 Production process and equipment of carbon black for rubber produced by using maltha
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
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
CN104694146A (en) * 2015-04-09 2015-06-10 河南开炭新材料有限公司 Flashing and pressure holding combined retention tower electric tracing heating temperature holding modified pitch production technology

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Application publication date: 20080220