CN101776547A - Method for easily and quickly evaluating needle coke - Google Patents
Method for easily and quickly evaluating needle coke Download PDFInfo
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- CN101776547A CN101776547A CN 201010100198 CN201010100198A CN101776547A CN 101776547 A CN101776547 A CN 101776547A CN 201010100198 CN201010100198 CN 201010100198 CN 201010100198 A CN201010100198 A CN 201010100198A CN 101776547 A CN101776547 A CN 101776547A
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Abstract
The invention relates to a method for easily and quickly evaluating needle coke. In the method, material to be evaluated is placed in a container, and the container is placed in a pyrolysis reactor; the temperature of the pyrolysis reactor is increased to 460 DEG C to 520 DEG C at the heating rate of 1 DEG C/min to 20 DEG C/min, and after the temperature is kept for one to two hours, the pyrolysis reactor is naturally cooled; the container is taken out of the pyrolysis reactor, and the material to be evaluated is taken out of the containing; the appearance of the coke is observed; if the coke is needle-like or fine strip-like particles, the material can be produced into needle coke; and if the coke is block-like, powder-like or block-like particles, the material cannot be produced into needle coke. The method can easily and quickly evaluate the feasibility of producing needle coke by certain material, an expensive instrument is not needed, the operation is simple, and professionals are not needed.
Description
Technical field
The present invention relates to a kind of method of simple quickly evaluating needle coke.
Background technology
Needle coke is a main material of producing ultra high power graphite electrode.Needle coke can be produced with the heavy distillate of petroleum refining and coal tar processing, and as thermal cracking residue, fluid catalytic cracking decant oil, coal-tar pitch etc., many rings (3～4 ring) aromatic hydrocarbons that is rich in short-side chain, line style connection is the quality raw materials of producing needle coke.Can be divided into coal-based needle coke to needle coke and oil is needle coke according to the difference of raw material sources.Requirement to needle-shape coke raw material on the commercial production is: arene content height (weight ratio is about 30%～50%), gum asphaltic content low (generally controlling heptane insolubles＜2.0%), ash content (general＜0.05) and sulphur content content low (being not more than 0.5%), vanadium and nickel content all are not more than 50ppm.Therefore on commercial production, estimate a kind of raw material and whether can produce needle coke and need carry out the series of analysis test, to obtain above-mentioned every index to this raw material.And above-mentioned analytical test process takes time and effort very much, also essential simultaneously professional tester and specialty and expensive testing apparatus.So method that is necessary to invent a kind of time saving and energy saving, simple and easy to do evaluation needle-shape coke raw material.
The purpose of this invention is to provide a kind of method that can quickly evaluating needle coke.
Main device of the present invention comprises box pyrolysis reactor, attemperating unit and holds the container of raw material to be evaluated.Operating process is: the container that will fill raw material to be evaluated is put into pyrolysis reactor, temperature of reactor is controlled by attemperating unit, from reactor, take out behind the raw material coking to be evaluated, estimate the feasibility that this raw material is produced needle coke by the outward appearance of observation post's coke.
Its concrete steps are as follows:
(1) raw material to be evaluated is placed container, and this container is placed pyrolysis reactor;
(2) the control pyrolysis reactor is warming up to 460-520 ℃ with heating rate 1-20 ℃/min, natural cooling after constant temperature 1-2 hour;
(3) after the pyrolysis reactor cooling, container is taken out from pyrolysis reactor, and raw material to be evaluated is taken out from container;
(4) outward appearance of observation coke, if coke is fine acicular or fine strip shape particle, then this raw material can be produced needle coke, if coke is bulk, powder or blocky-shaped particle, then this raw material can not be produced needle coke.
Aforesaid raw material to be evaluated is that coal measures raw material, oil are that raw material or oil are the coal measures mixed material.The coal measures raw material is coal tar, dead oil or coal-tar asphalt.Oil is that raw material is black petroleum products, ethylene bottom oil, catalytic cycle oil, coking recycle oil.
Container of the present invention is a small containers with cover, as ceramic crucible.
Pyrolysis reactor of the present invention is a box type furnace, as muffle furnace.
The present invention has following advantage:
1, can estimate the feasibility that certain raw material is produced needle coke simply fast;
2, time saving and energy saving, simple to operate, need not expensive instrument and full-time staff.
Description of drawings
Fig. 1 is the outward appearance photo of 1 coking of embodiment.
Fig. 2 is the outward appearance photo of 2 cokings of embodiment.
Fig. 3 is the outward appearance photo of 3 cokings of embodiment.
Fig. 4 is the outward appearance photo of 4 cokings of embodiment.
Fig. 5 is the outward appearance photo of 5 cokings of embodiment.
Fig. 6 is the outward appearance photo of 6 cokings of embodiment.
Fig. 7 is the outward appearance photo of 7 cokings of embodiment.
Fig. 8 is the outward appearance photo of 8 cokings of embodiment.
Embodiment
Embodiment 1
The 20ml catalytic cycle oil is placed crucible with cover, should put into muffle furnace by crucible with cover, muffle furnace under attemperating unit control by room temperature temperature programme to 500 ℃, and at 500 ℃ of following constant temperature one hour, 3 ℃/min of heating rate.The oil sample that is placed in the crucible is accompanied by the temperature-rise period generation pyrogenetic reaction of muffle furnace, and finally generates coke.With coke took out and observed coke from crucible outward appearance (coke outward appearance photo is seen Fig. 1, ratio 1: 1), as can be seen, this coke outward appearance is the fine acicular particle, illustrates that this catalytic cycle oil can produce needle coke.
Embodiment 2
The 30ml coking recycle oil is placed crucible with cover, should put into muffle furnace by crucible with cover, muffle furnace under attemperating unit control by room temperature temperature programme to 480 ℃, and at 480 ℃ of following constant temperature one hour, 10 ℃/min of heating rate.The oil sample that is placed in the crucible is accompanied by the temperature-rise period generation pyrogenetic reaction of muffle furnace, and finally generates coke.With coke took out and observed coke from crucible outward appearance (coke outward appearance photo is seen Fig. 2, ratio 1: 1), as can be seen, this coke outward appearance is the fine acicular particle, illustrates that this coking recycle oil can produce needle coke.
Embodiment 3
50ml coal tar is placed crucible with cover, should put into muffle furnace by crucible with cover, muffle furnace under attemperating unit control by room temperature temperature programme to 490 ℃, and at 490 ℃ of following constant temperature one hour, 20 ℃/min of heating rate.The oil sample that is placed in the crucible is accompanied by the temperature-rise period generation pyrogenetic reaction of muffle furnace, and finally generates coke.With coke took out and observed coke from crucible outward appearance (coke outward appearance photo is seen Fig. 3, ratio 1: 1), as can be seen, this coke outward appearance is tiny bulk, illustrates that this coal tar can not produce needle coke.
Embodiment 4
The potpourri (1: 1) of 40ml black petroleum products and coal tar is placed crucible with cover, should put into muffle furnace by crucible with cover, muffle furnace under attemperating unit control by room temperature temperature programme to 470 ℃, and at 470 ℃ of following constant temperature one hour, 2 ℃/min of heating rate.Be placed on the heavy oil in the crucible and the potpourri sample of coal-tar pitch and be accompanied by the temperature-rise period generation pyrogenetic reaction of muffle furnace, and finally generate coke.With coke took out and observed coke from crucible outward appearance (coke outward appearance photo is seen Fig. 4, ratio 1: 1), as can be seen, this coke outward appearance is fine acicular or fine strip shape particle, illustrates that this black petroleum products can produce needle coke.
Embodiment 5
The 30ml black petroleum products is placed crucible with cover, should put into muffle furnace by crucible with cover, muffle furnace under attemperating unit control by room temperature temperature programme to 460 ℃, and at 460 ℃ of following constant temperature two hours, 1 ℃/min of heating rate.The oil sample that is placed in the crucible is accompanied by the temperature-rise period generation pyrogenetic reaction of muffle furnace, and finally generates coke.With coke took out and observed coke from crucible outward appearance (coke outward appearance photo is seen Fig. 5, ratio 1: 1), as can be seen, this coke outward appearance is smalls shape or tiny blocky-shaped particle, illustrates that this black petroleum products can not produce needle coke.
Embodiment 6
The 40ml coal-tar asphalt is placed crucible with cover, should put into muffle furnace by crucible with cover, muffle furnace under attemperating unit control by room temperature temperature programme to 520 ℃, and at 520 ℃ of following constant temperature one hour, 3 ℃/min of heating rate.The coal-tar pitch that is placed in the crucible is accompanied by the temperature-rise period generation pyrogenetic reaction of muffle furnace, and finally generates coke.Coke was taken out and observed coke from crucible outward appearance (coke outward appearance photo is seen Fig. 6, ratio 1: 1), as can be seen, it is block that this coke outward appearance is, and illustrates that this coal-tar pitch can not produce needle coke.
Embodiment 7
The 40ml ethylene bottom oil is placed crucible with cover, should put into muffle furnace by crucible with cover, muffle furnace under attemperating unit control by room temperature temperature programme to 470 ℃, and at 470 ℃ of following constant temperature two hours, 2 ℃/min of heating rate.The oil sample that is placed in the crucible is accompanied by the temperature-rise period generation pyrogenetic reaction of muffle furnace, and finally generates coke.With coke took out and observed coke from crucible outward appearance (coke outward appearance photo is seen Fig. 7, ratio 1: 1), as can be seen, this coke outward appearance is fine acicular or fine strip shape particle, illustrates that this ethylene bottom oil can produce needle coke.
Embodiment 8
The potpourri (2: 1) of 30ml dead oil and ethylene bottom oil is placed crucible with cover, should put into muffle furnace by crucible with cover, muffle furnace under attemperating unit control by room temperature temperature programme to 500 ℃, and at 500 ℃ of following constant temperature one hour, 3 ℃/min of heating rate.The oil sample that is placed in the crucible is accompanied by the temperature-rise period generation pyrogenetic reaction of muffle furnace, and finally generates coke.With coke took out and observed coke from crucible outward appearance (coke outward appearance photo is seen Fig. 8, ratio 1: 1), as can be seen, this coke outward appearance is smalls shape or tiny blocky-shaped particle, illustrates that the potpourri of this dead oil and ethylene bottom oil can not be produced needle coke.
Claims (7)
1. the method for an easy quickly evaluating needle coke is characterized in that comprising the steps:
(1) raw material to be evaluated is placed container, and this container is placed pyrolysis reactor;
(2) the control pyrolysis reactor is warming up to 460-520 ℃ with heating rate 1-20 ℃/min, natural cooling after constant temperature 1-2 hour;
(3) after the pyrolysis reactor cooling, container is taken out from pyrolysis reactor, and raw material to be evaluated is taken out from container;
(4) outward appearance of observation coke, if coke is fine acicular or fine strip shape particle, then this raw material can be produced needle coke, if coke is bulk, powder or blocky-shaped particle, then this raw material can not be produced needle coke.
2. the method for a kind of easy quickly evaluating needle coke as claimed in claim 1 is characterized in that described raw material to be evaluated is that coal measures raw material, oil are that raw material or oil are the coal measures mixed material.
3. the method for a kind of easy quickly evaluating needle coke as claimed in claim 2 is characterized in that described coal measures raw material is coal tar, dead oil or coal-tar asphalt.
4. the method for a kind of easy quickly evaluating needle coke as claimed in claim 2 is characterized in that described oil is that raw material is black petroleum products, ethylene bottom oil, catalytic cycle oil or coking recycle oil.
5. the method for this a kind of easy quickly evaluating needle coke as claimed in claim 1 is characterized in that described container is a ceramic crucible.
6. the method for a kind of easy quickly evaluating needle coke as claimed in claim 1 is characterized in that described pyrolysis reactor is a box type furnace.
7. the method for a kind of easy quickly evaluating needle coke as claimed in claim 6 is characterized in that described box type furnace is a muffle furnace.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101001982A CN101776547B (en) | 2010-01-20 | 2010-01-20 | Method for easily and quickly evaluating needle coke |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010101001982A CN101776547B (en) | 2010-01-20 | 2010-01-20 | Method for easily and quickly evaluating needle coke |
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| CN101776547A true CN101776547A (en) | 2010-07-14 |
| CN101776547B CN101776547B (en) | 2011-06-08 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102435605A (en) * | 2011-09-19 | 2012-05-02 | 中国石油天然气股份有限公司 | Method for optimizing outlet temperature of delayed coking heating furnace |
| CN107194915A (en) * | 2017-04-21 | 2017-09-22 | 重庆交通大学 | The evaluation method of deleterious particle in aggregate particle |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4547284A (en) * | 1982-02-16 | 1985-10-15 | Lummus Crest, Inc. | Coke production |
| 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 |
| CN1143888C (en) * | 2000-03-24 | 2004-03-31 | 上海宝钢化工有限公司 | Preparation method of coal series needle type coke |
| CN1169911C (en) * | 2001-11-14 | 2004-10-06 | 中国科学院山西煤炭化学研究所 | Method for preparing needle coke |
| CN100549141C (en) * | 2005-05-31 | 2009-10-14 | 中国石油化工股份有限公司 | A kind of preprocessing method of raw materials of producing needle coke |
-
2010
- 2010-01-20 CN CN2010101001982A patent/CN101776547B/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102435605A (en) * | 2011-09-19 | 2012-05-02 | 中国石油天然气股份有限公司 | Method for optimizing outlet temperature of delayed coking heating furnace |
| CN107194915A (en) * | 2017-04-21 | 2017-09-22 | 重庆交通大学 | The evaluation method of deleterious particle in aggregate particle |
| CN107194915B (en) * | 2017-04-21 | 2020-07-10 | 重庆交通大学 | Method for evaluating harmful particles in aggregate particles |
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| Publication number | Publication date |
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| CN101776547B (en) | 2011-06-08 |
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Inventor after: Guo Shaoqing Inventor after: Zhao Liangfu Inventor after: Zhang Ye Inventor after: Qiu Zegang Inventor after: Zhu Hongying Inventor after: Li Zhenrong Inventor after: Zhang Wei Inventor after: Wang Guiyun Inventor before: Zhao Liangfu Inventor before: Guo Shaoqing Inventor before: Zhang Ye Inventor before: Qiu Zegang Inventor before: Zhu Hongying Inventor before: Li Zhenrong |
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Free format text: CORRECT: INVENTOR; FROM: ZHAO LIANGFU GUO SHAOQING ZHANG YE QIU ZEGANG ZHU HONGYING LI ZHENRONG TO: GUO SHAOQING ZHAO LIANGFU ZHANG YE QIU ZEGANG ZHU HONGYING LI ZHENRONG ZHANG WEI WANG GUIYUN |
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Granted publication date: 20110608 Termination date: 20170120 |