CN1418930A - Method for preparing needle coke using petrolium and coal series raw material - Google Patents
Method for preparing needle coke using petrolium and coal series raw material Download PDFInfo
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- CN1418930A CN1418930A CN 01140586 CN01140586A CN1418930A CN 1418930 A CN1418930 A CN 1418930A CN 01140586 CN01140586 CN 01140586 CN 01140586 A CN01140586 A CN 01140586A CN 1418930 A CN1418930 A CN 1418930A
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Abstract
The method for preparing needle coke by using petroleum system raw material and coal system raw material includes the following steps: firstly, mixing the petroleum system raw material and coal system raw material according to the weight ratio of 1:0.1-10; heat-treating for 0.5-4h at 400-440 deg.C and 0.2-2 MPa in inert gas atmosphere; heating to 490-550 deg.c within 2-30 sec., then coking for 3-8 h. at 0.2-2 MPa. Its yield rate is high, and its optical structure is good.
Description
Technical field:
The invention belongs to a kind of method for preparing needle coke, relate in particular to a kind of method with oil system and coal measures feedstock production needle coke.
Background technology:
Needle coke is a main raw material of producing ultra-high power graphite electrode.According to raw material sources, needle coke can be divided into oil system and coal measures two big classes.Although the production technique of the two is not quite similar, purposes is identical basically.
Coal measures raw material such as coal tar and pitch thereof are applied with needle coke as the common superpower electrode of preparation, and its constructional feature is that aromaticity is higher, and alkyl group side chain is few, contains alicyclic structure hardly; Oil is that raw material such as catalytic slurry then contain more aliphatic side chains and abundant cycloalkanes structure.This shows that the structure of two class raw materials is obviously different.The two independent coking, high to ingredient requirement, and be difficult for making the higher needle coke of performance.If their will be carried out coking after directly mixing, then in pyrolytic process because the relatively poor separation that will cause phase and phase of consistency, finally cause the system reaction inhomogeneous and produce pattern structure, thereby can't prepare the needle coke of better performances.
Yield is higher after the coking of coal measures raw material, and the rich coal resources of China, but its constructional feature has determined its direct coking to be difficult for making the more excellent needle coke of performance; And that oil is the coking yield of raw material is lower, and china natural resources is also relatively deficienter, moreover its constructional feature also shown it in the difficulty aspect the starting raw material of needle coke, so these two kinds of independent coking of raw material are difficult for making the higher needle coke of performance.But, if utilize the advantage of the two structure, will charing altogether behind the two thorough mixing, coking more afterwards then can make the needle coke of excellent performance.This will be significant to the production of China's needle coke.But up to the present, only limit in the document use homogeneous raw material to prepare needle coke, as at document Fuel (1978,57:225-231), be after petroleum pitch is used the benzene extracting and separating, the composition that obtains being dissolved in benzene (BS) and be insoluble to benzene (BI) directly carries out coking after then BS and BI being mixed by a certain percentage.Because what adopt is with a kind of bituminous heterogeneity,, finally make optical texture needle coke preferably so intermiscibility is better during coking; At document Carbon (1989,27:359-380), be directly to carry out coking after having selected for use two kinds of petroleum residual oils to mix mutually to prepare needle coke, because what select for use is the petroleum residual oil that structure and composition are more or less the same, thereby the intermiscibility of the two is better, has finally also obtained optical texture needle coke preferably.
Goal of the invention:
The method that the purpose of this invention is to provide a kind of oil system and coal measures feedstock production needle coke.
Principle of the present invention is as follows: must satisfy three conditions during the preparation needle coke, i.e. good, the modest viscosity of intermediate phase and the disengaging of relatively large gas in flakes of anisotropy development.Coal measures raw material aromaticity is higher, when coking, do not react hardly because of reaching the required activation energy of reaction under the lesser temps, nearly all molecule has all had the required activation energy of reaction again when comparatively high temps, thereby certainly will form a plurality of reactive centers in the system, and too much the existence of reactive center makes polycondensation become restive, it has contained the alicyclic structure of hydrogenation hardly in addition, make reaction stability relatively poor, system viscosity is higher, thereby and can't disengaging more amount gas, aliphatic side chains seldom make intermediate phase that co-axial orientation can not take place, so be difficult for making needle coke; Oil is that the raw material aromaticity is lower, contain a large amount of aliphatic side chainses and alicyclic structure, like this, in reaction process, certainly will resemble and form too much reactive center the coal measures raw material, make the intermediate phase spherocrystal have little time fully to grow up after generating and promptly melt and form thin pattern structure mutually.So also be difficult for making needle coke; If with oil is to carry out coking after raw material and coal measures raw material directly mix, then because the two molecular structure differs greatly, and consistency is relatively poor when coking, the speed of response difference causes phase and phase to separate, and finally also can't make needle coke.Therefore must solve the two compatibility problem.The present invention proposes that the two is mixed the back and heat-treats being lower than under the coking temperature, so that both contained the fragrant ingredient that forms intermediate phase in the two reacted product structure, the aliphatic side chains that contains simultaneously appropriateness again needed gas when obtaining the intermediate phase orientation, also contain alicyclic structure in addition with the reduction system viscosity, thereby solved the compatibility problem of different material.
A kind of method with oil system and coal measures feedstock production needle coke of the present invention is as follows:
(1) at first with oil system and coal measures raw material with 1: the weight ratio of 0.1-10 is mixed mutually, 400-440 ℃ with 0.2-2MPa under in inert gas atmosphere thermal treatment 0.5-8h;
(2) be warmed up to 490-550 ℃ in time second at 2-30, then coking 3-8h under 0.2-2MPa.
Aforesaid coal measures raw material is coal tar and a coal-tar pitch of removing the objectionable constituent quinoline insolubles.
Aforesaid oil is that raw material is black petroleum products, ethylene bottom oil, catalytic cracking residual oil and thermal cracking residue etc.
Aforesaid rare gas element is N
2, Ar etc.
Characteristics of the present invention are:
(1) by a certain percentage two kinds of raw materials of blended through Overheating Treatment or copolymerization, thereby change the two intermiscibility;
(2) can obtain the higher and optical texture of coking yield needle coke preferably;
(3) make full use of coal tar and petroleum resources, improve the scientific and technological added value of coal tar.
(4) the present invention prepares simple, easy to operate.
Embodiment:
Embodiment 1:
The supercritical extraction slurry oil 3kg and the coal measures flash oil 2kg that originate from the Liaohe River mix, charing 5h altogether under 425 ℃, 0.8MPa then, gained pitch is coking 8h under 510 ℃/1.5MPa, its optical texture is seen Fig. 1, can find out does not have pattern structure to produce, whole coke button is mainly melted greatly by thick wide area and the streamline structure of body is formed, and degree of orientation is higher, is suitable as the starting raw material of needle coke preparation.
Comparative Examples 1:
Direct coking 8h under 510 ℃/1.5MPa after originating from the supercritical extraction slurry oil 3kg in the Liaohe River and coal measures flash oil 2kg and mixing, its optical texture is seen Fig. 2, can find out in whole burnt body to have more pattern structure, belongs to the needle coke of poor-performing.
Embodiment 2:
The supercritical extraction slurry oil 1kg and the coal measures flash oil 4kg that originate from grand celebration mix, charing 8h altogether under 400 ℃, 0.2MPa then, gained pitch is coking 3h under 550 ℃/2MPa, its optical texture is seen Fig. 3, can find out does not have pattern structure to produce, whole coke button is made up of the higher streamline structure of degree of orientation, is a needle coke preferably.
Comparative Examples 2:
Direct coking 3h under 550 ℃/2MPa after originating from the supercritical extraction slurry oil 1kg of grand celebration and coal measures flash oil 4kg and mixing, its optical texture is seen Fig. 4, can find out in whole burnt body to have more pattern structure gained needle coke poor-performing.
Embodiment 3:
Petroleum residual oil 1kg and coal tar 5kg mix, thermal treatment 0.5h under 440 ℃, 1.6MPa then, gained pitch is coking 6h under 490 ℃/0.2MPa, its optical texture is seen Fig. 5, can find out does not have pattern structure to produce, whole coke button mainly is made up of the streamline structure of higher degree of orientation, is a good needle coke.
Comparative Examples 3:
Petroleum residual oil 1kg and coal tar 5kg mix, direct coking 6h under 490 ℃/0.2MPa then, and its optical texture is seen Fig. 6, can find out in burnt body it mainly is pattern structure, gained needle coke poor performance.
Embodiment 4:
The flash oil that originates from Anshan behind thermal polycondensation under the 400 ℃/0.5MPa product 8kg and mix based on the cured matter residual oil 1kg of aliphatic hydrocarbon, thermal treatment 4h under 440 ℃, 1.6MPa then, gained pitch is coking 5h under 490 ℃/0.5MPa, its optical texture is seen Fig. 7, can find out that coke button is made up of the higher wide area structure of degree of orientation, be a needle coke preferably.
Comparative Examples 4:
The polycondensate of flash oil and directly mixed back coking 5h under 490 ℃/0.5MPa with 8: 1 based on the cured matter residual oil of aliphatic hydrocarbon, its optical texture is seen Fig. 8, can find out at Jiao Tizhong to have pattern structure, is difficult for making the needle coke of better performances.
Embodiment 5:
The higher catalytic cracking residual oil 3kg of coal tar 1kg and aromaticity mixes, thermal treatment 3h under 440 ℃, 1.0MPa then, and gained pitch is coking 6h under 510 ℃/1.5MPa, and its optical texture is seen Fig. 9, can find out that coke button is a needle coke preferably.
Comparative Examples 5:
Coal tar with directly mixed back coking 6h under 510 ℃/1.5MPa with the higher catalytic cracking residual oil of aromaticity with 1: 3, its optical texture is seen Figure 10, can find out that coke button is a relatively poor needle coke.
Claims (4)
1. method with oil system and coal measures feedstock production needle coke, its characteristics are:
(1) at first with oil system and coal measures raw material with 1: the weight ratio of 0.1-10 is mixed mutually, 400-440 ℃ with 0.2-2MPa under in inert atmosphere thermal treatment 0.5-8h;
(2) be warmed up to 490-550 ℃ in time second at 2-30, then coking 3-8h under 0.2-2MPa.
2. a kind of method with oil system and coal measures feedstock production needle coke as claimed in claim 1 is characterized in that described coal measures raw material is coal tar and a coal-tar pitch of removing the objectionable constituent quinoline insolubles.
3. a kind of method with oil system and coal measures feedstock production needle coke as claimed in claim 1 is characterized in that described oil is that raw material is black petroleum products, ethylene bottom oil, catalytic cracking residual oil and thermal cracking residue.
4. a kind of method with oil system and coal measures feedstock production needle coke as claimed in claim 1 is characterized in that described rare gas element is N
2Or Ar.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 01140586 CN1418930A (en) | 2001-11-14 | 2001-11-14 | Method for preparing needle coke using petrolium and coal series raw material |
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| CN 01140586 CN1418930A (en) | 2001-11-14 | 2001-11-14 | Method for preparing needle coke using petrolium and coal series raw material |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101942314A (en) * | 2009-07-09 | 2011-01-12 | 中国石油化工股份有限公司抚顺石油化工研究院 | Technology for producing needle coke by kettle-type coking |
| CN102041011A (en) * | 2009-10-16 | 2011-05-04 | 中国石油化工股份有限公司 | Method for preparing needle coke through still coking |
| CN101353236B (en) * | 2008-09-12 | 2012-09-05 | 中国海洋石油总公司 | Asphalt modifying agent and preparation thereof |
| CN102965132A (en) * | 2012-08-23 | 2013-03-13 | 方大炭素新材料科技股份有限公司 | Method for preparing needle coke by magnetization reaction kettle |
| CN103102890A (en) * | 2011-11-10 | 2013-05-15 | 中国石油化工股份有限公司 | Process method for preparing needle coke through kettle type charring |
| CN103965932A (en) * | 2014-04-30 | 2014-08-06 | 上海宝聚新化能源科技有限公司 | Treatment method for mixed asphalt as raw material for preparing needle coke |
| CN103965928A (en) * | 2014-04-30 | 2014-08-06 | 上海宝聚新化能源科技有限公司 | Coking method for coal-oil mixed pitch |
| CN104232130A (en) * | 2013-06-09 | 2014-12-24 | 任相坤 | Process of producing needle coke |
| CN109943354A (en) * | 2019-03-29 | 2019-06-28 | 山东益大新材料有限公司 | A kind of Co carbonization technique of aromatic naphtha and refined bitumen mixed raw material |
| CN113773870A (en) * | 2021-08-31 | 2021-12-10 | 山东常任新材料有限公司 | Preparation method of mesophase pitch |
-
2001
- 2001-11-14 CN CN 01140586 patent/CN1418930A/en active Pending
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101353236B (en) * | 2008-09-12 | 2012-09-05 | 中国海洋石油总公司 | Asphalt modifying agent and preparation thereof |
| CN101942314A (en) * | 2009-07-09 | 2011-01-12 | 中国石油化工股份有限公司抚顺石油化工研究院 | Technology for producing needle coke by kettle-type coking |
| CN101942314B (en) * | 2009-07-09 | 2013-04-10 | 中国石油化工股份有限公司 | Technology for producing needle coke by kettle-type coking |
| CN102041011A (en) * | 2009-10-16 | 2011-05-04 | 中国石油化工股份有限公司 | Method for preparing needle coke through still coking |
| CN102041011B (en) * | 2009-10-16 | 2014-08-20 | 中国石油化工股份有限公司 | Method for preparing needle coke through still coking |
| CN103102890B (en) * | 2011-11-10 | 2014-04-16 | 中国石油化工股份有限公司 | Process method for preparing needle coke through kettle type charring |
| CN103102890A (en) * | 2011-11-10 | 2013-05-15 | 中国石油化工股份有限公司 | Process method for preparing needle coke through kettle type charring |
| CN102965132A (en) * | 2012-08-23 | 2013-03-13 | 方大炭素新材料科技股份有限公司 | Method for preparing needle coke by magnetization reaction kettle |
| CN104232130A (en) * | 2013-06-09 | 2014-12-24 | 任相坤 | Process of producing needle coke |
| CN104232130B (en) * | 2013-06-09 | 2016-08-10 | 任相坤 | A kind of production technology of needle coke |
| CN103965932A (en) * | 2014-04-30 | 2014-08-06 | 上海宝聚新化能源科技有限公司 | Treatment method for mixed asphalt as raw material for preparing needle coke |
| CN103965928A (en) * | 2014-04-30 | 2014-08-06 | 上海宝聚新化能源科技有限公司 | Coking method for coal-oil mixed pitch |
| CN103965932B (en) * | 2014-04-30 | 2016-02-10 | 上海宝聚新化能源科技有限公司 | As the treatment process of the mix asphalt of needle-shape coke raw material |
| CN109943354A (en) * | 2019-03-29 | 2019-06-28 | 山东益大新材料有限公司 | A kind of Co carbonization technique of aromatic naphtha and refined bitumen mixed raw material |
| CN113773870A (en) * | 2021-08-31 | 2021-12-10 | 山东常任新材料有限公司 | Preparation method of mesophase pitch |
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