CN1872963A - Method of treating raw material for producing acerate coke - Google Patents
Method of treating raw material for producing acerate coke Download PDFInfo
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- CN1872963A CN1872963A CN 200510073095 CN200510073095A CN1872963A CN 1872963 A CN1872963 A CN 1872963A CN 200510073095 CN200510073095 CN 200510073095 CN 200510073095 A CN200510073095 A CN 200510073095A CN 1872963 A CN1872963 A CN 1872963A
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Abstract
This invention discloses a method for pretreating the oil raw material for producing needle-like coke. The method comprises: (1) distilling the oil raw material to remove the unideal components; (2) contacting the ideal components with hydrogen and the hydrogenating catalyst, and separating the hydrogenated products to obtain the raw material for producing needle-like coke. The method can remove the unideal components from the oil raw material by combination of the two techniques, thus can rationally utilize hydrogen, save the cost, and largely reserve the ideal components.
Description
Technical field
The multistep process method that the invention belongs to a kind of hydrocarbon ils distillation and make with extra care hydrocarbon ils with hydrogen more particularly, is a kind of preprocessing method of raw materials of producing needle coke.
Technical background
Needle coke has that thermal expansivity (CTE) is low, crystallization degree is high, the electric conductivity advantages of higher, and the hole in the coke button is evenly directed, is elongated oval shape.Needle coke can have been widely used in industry, national defence, medical treatment and space industry as the important source material of producing ultra high power and high power graphite electrode.The output of China's needle coke (green coke) is about 1.5 ten thousand tons at present, can't satisfy the demand, and still needs about 4.5 ten thousand tons of import needle coke (ripe Jiao).Although it is the product of delayed coking process, compare with producing general Jiao, raw material and technology there are special requirement.At first the burnt production technology of pin is the mesophasespherule formation mechanism, and colloid and bituminous matter are the macromole fused ring compounds that has long side chain, can hinder the generation of fine-fibered shape structure needle coke; Secondly the sulphur content among pin Jiao must be low, because graphitizing furnace child-operation extreme temperatures, typical graphitization temperature is approximately 2800 ℃, so in graphitizing process, be accompanied by the effusion of sulphur, puffing takes place, finally make Graphite Electrodes intensity be subjected to grievous injury.
According to the character and the formation mechanism of needle coke, aspect raw material, should select the raw material of low-sulfur, low bituminous matter, low colloid and low ash content, generally adopt fluid catalytic cracking decant oil, thermal cracking residue etc.But most of oil plants all exist variety of problems in these raw materials, such as bituminous matter, colloid and grey grade foreign matter content height and the high problem of sulfur-bearing.If can not handle these problems timely and effectively, the raw material of producing pin Jiao just is very restricted, thereby also just can't satisfy large-scale industrial production, and can't produce qualified needle coke.Therefore the raw material that how to obtain qualified production pin Jiao is the problem that people study always.
US4178229 discloses the method that a kind of straight run vacuum residuum is produced high-quality petroleum coke, earlier vacuum residuum is converted into distillate and pitch, more further with pitch and hydrogen supply agent cracking production high-quality Jiao's raw material.
US4235703 discloses a kind of method with residual oil production high-quality Jiao, and this method is produced superpower electrode refinery coke through delay coking process with raw material earlier again after hydrogenating desulfurization, demetalization.
US4894144 discloses a kind of method for preparing needle coke and high sulfur petroleum coke simultaneously, and it adopts hydroprocessing technique that straight run heavy oil is carried out pre-treatment, and the residual oil separated into two parts that hydrogenation is crossed is calcined after coking respectively again and made needle coke and high sulfur petroleum coke.
US5286371 also discloses the straight run residue hydroprocessing technique, 379～480 ℃ of hydrogenation reaction temperature, reaction pressure 6.8MPa～34.4MPa, heavy residual oil and the fluid catalytic cracking decant oil handled are mixed into solvent deasphalting unit, remove logistics behind the pitch as the raw material of needle coke.
CN1325938A discloses a kind of method of producing acicular petroleum coke with sulfur containing atmospheric, after raw material passes through hydrofining, hydrodemetallation (HDM), hydrogenating desulfurization successively in this this method, the hydrogenation heavy distillate that the separation hydrogenated oil obtains enters delayed coking unit, under the condition of producing pin Jiao, obtain pin Jiao, hydrofining is 350～420 ℃ of temperature of reaction, hydrogen dividing potential drop 5.0～22.0MPa, hydrogen-oil ratio 500～1200Nm
3/ m
3Condition under react.
The subject matter that above-mentioned prior art exists is, undesirable components bituminous matter in the stock oil and colloid etc. are not removed but participate in hydrogenation process, hydrogen is not effectively utilized, and higher because of the severity of hydrogenation, causes the ideal composition aromatic hydrocarbons loss in the stock oil.
Summary of the invention
The objective of the invention is on the prior art basis, to provide a kind of preprocessing method of raw materials of producing needle coke, to remove the undesirable components in the stock oil, keep the ideal composition aromaticity content not reduce simultaneously, make the stock oil after the processing satisfy the requirement of producing needle-shape coke raw material.
The preprocessing method of raw materials of production needle coke provided by the invention comprises:
Stock oil removes wherein undesirable components through underpressure distillation earlier, and remaining ideal composition contacts with hydrogen, hydrogenation catalyst, and the hydrogenation reaction logistics obtains producing the raw material of needle coke through separation.
Method of the present invention can remove light, the heavy undesirable components in the stock oil by the combination of two kinds of technologies, and reasonable use hydrogen has been saved investment more, keeps ideal composition to greatest extent, and the stock oil after the processing satisfies the requirement of producing needle-shape coke raw material.
Description of drawings
Accompanying drawing is the preprocessing method of raw materials synoptic diagram of production needle coke provided by the invention.
Embodiment
Method provided by the invention is so concrete enforcement:
Stock oil is earlier successively by filtering and underpressure distillation removes lightweight undesirable components such as heavy undesirable components such as bituminous matter, colloid and part of ash and diesel oil distillate, wherein the lightweight undesirable components is extracted out from decompression cat head and vacuum 1st side cut, the heavy undesirable components is extracted out at the bottom of tower, the extraction from tower of remaining ideal composition contacts with hydrogen, hydrogenation catalyst, and the hydrogenation reaction logistics obtains producing the raw material of needle coke through separation.
Stock oil of the present invention is selected from one or more in heavy distillate, catalytically cracked oil or clarified oil, steam cracking residual oil, the thermal cracking residue, and wherein heavy distillate is the wax oil cut, and its boiling range is 270～500 ℃.The sulphur content of stock oil is greater than 0.6 heavy %, and sulphur content is high more in the stock oil that the present invention relates to shows technical superiority of the present invention more.If stock oil is catalytically cracked oil or clarified oil, must to remove catalyst fines, reduce ash content earlier to its filtration; If stock oil is heavy distillate, steam cracking residual oil, thermal cracking residue, then needn't be earlier to its filtration.
Filtration condition of the present invention is pressure 0.2～5.0MPa, 40～350 ℃ of temperature.
Underpressure distillation of the present invention is one or more levels distillation, and operational condition is pressure 5mmHg～100mmHg, 300～450 ℃ of temperature.The ideal composition boiling range that obtains through underpressure distillation is: 5% is not less than 380 ℃, and 95% is not more than 485 ℃.Wherein the imperfect cut of heavy, lightweight undesirable components and ideal composition account for 10～15%, 0～5%, 80%～90% of stock oil respectively.
The characteristics of hydrogenation reaction desulfurization of the present invention are high-temperature low-pressures, and purpose is to remove sulphur, keeps its aromaticity content simultaneously.Reactor adopts fixed bed, and the activity of hydrocatalyst component is metal, metal oxide, the metallic sulfide of VIB, VIIB, VIIIB family element, and wherein the group vib element is Mo, W, and VIIB family element is Mn, and VIIIB family element is Ni, Co, Fe.Temperature of reaction is 300～420 ℃, and reaction pressure is 1.5-5.0MPa, and hydrogen-oil ratio is 50～500Nm
3/ m
3, volume space velocity 0.5～5h
-1The stock oil desulfurization degree reaches 30～70%.
By adding cold residual oil to reduce column bottom temperature, prevent the viscosity of coking and reduction bottoms material at the bottom of the decompression Tata, the cold residue oil temperature of described mistake is 100～350 ℃, and mixed heavy residual oil is extracted out as the raw material of producing ordinary coke as bottom product.
The present invention has utilized the combination process of filtering system, underpressure distillation, mild hydrogenation to realize pre-treatment to the burnt raw material of pin.At first remove ash content through filtering system, remove heavy undesirable components such as bituminous matter, colloid and part of ash and lightweight undesirable components such as diesel oil lighting end by reduced pressure distillation process then, owing to be rich in short-side chain, the polycyclic aromatic hydrocarbons that 3～4 rings are arranged is a good raw material of producing needle coke, therefore sets vacuum 1st side cut and extracts low weight component out.80%～90% stock oil is extracted out from the centre, mild hydrogenation again, and its hydrogenation degree of depth need not reach the degree of depth of residual hydrogenation.The combination of the present invention by two kinds of technologies can remove the weight undesirable components in the stock oil, this than first hydrogenation after the combination process reasonable use hydrogen more of solvent deasphalting, saved investment, purifying and keep ideal composition to greatest extent.
Below in conjunction with accompanying drawing method provided by the present invention further is illustrated, the underpressure distillation in the inventive method is the one-level distillation, but is not limited to the one-level distillation, and multistage distillation also is applicable to the present invention.
Accompanying drawing is the preprocessing method of raw materials synoptic diagram of production needle coke provided by the invention, has omitted the equipment of many necessity such as pump etc. among the figure.
Stock oil enters surge tank 4 through pipeline 1, and by entering filtering system through pipeline 5 earlier after the pump supercharging, the raw material after the filtration is in the radiation section heating of process furnace 6.Stock oil enters into vacuum distillation tower 8 through pipeline 7 subsequently, and vacuum distillation tower 8 required stripped vapors enter at the bottom of tower.Cause in the tower coking in order to prevent reaction such as residual oil decomposes at the bottom of the tower, condensation or can't discharge greatly, at the bottom of tower, introduced cold vacuum residuum, reduce the tendency that residual oil decomposes coking to reduce column bottom temperature through pipeline 3 because of viscosity.Cat head oil gas is drawn through pipeline 9, is provided with the pump around circuit system on vacuum distillation tower top, and logistics is pumped out at the 3rd block of column plate, gets back to cat head by heat exchange cooling back one tunnel, and extract out through pipeline 10 as vacuum 1st side cut on another road.After stock oil after the underpressure distillation is pumped out and mixes from the recycle hydrogen of pipeline 11, enter process furnace 16 through pipeline 12, in process furnace 16, stock oil is heated to 300～420 ℃ of temperature of reaction, enter hydrogenator 13 then and carry out the mild hydrogenation desulfurization, stock oil cooling back after refining is separated into vapour, liquid two-phase to high pressure separating tank 17, wherein gas phase is compressed the back by hydrogen compressor 20 and is used from the new hydrogen mixed cycle of pipeline 19, and the burnt raw material of qualified pin arrives the burnt technological process of production of pin by pipeline 18.
The following examples will give further instruction to present method, but therefore not limit present method.
Utilize method processing of the present invention catalysis clarified oil as shown in table 1, filtration condition is pressure 1.0MPa (gauge pressure), 250 ℃ of temperature; The underpressure distillation operational condition is pressure 20mmHg, 400 ℃ of heater outlet temperatures, and the underpressure distillation material distributes as shown in table 2; The activity of hydrocatalyst component is Ni, W.The hydrogenation reaction temperature is 380 ℃, and the reactive hydrogen dividing potential drop is 2.5MPa, and hydrogen-oil ratio is 300Nm
3/ m
3, volume space velocity 0.8h
-1
Experimental result sees Table 1, and the data of contrast table 1 and table 3 can make the catalysis clarified oil satisfy the requirement of the burnt raw material of pin as can be known by behind filtration, underpressure distillation, the mild hydrogenation.
The refining front and back of catalysis clarified oil change of properties table in table 1, the raw material pretreatment process
| The oil product title | The catalysis clarified oil | Clarified oil after the underpressure distillation | The burnt raw material of pin |
| Density (20 ℃), g/cm 3 | 1.0486 | 1.0384 | 1.0323 |
| Kinematic viscosity (80 ℃), mm 2/s | 159.32 | 78.23 | 78.24 |
| Kinematic viscosity (100 ℃), mm 2/s | 50.04 | 26.52 | 26.54 |
| Carbon residue, m% | 12.28 | 6.16 | 6.16 |
| Ash content, m% | 0.116 | 0.008 | 0.003 |
| Ultimate analysis, m% | |||
| C | 90.20 | 90.10 | 90.10 |
| H | 8.35 | 8.74 | 9.30 |
| S | 1.18 | 0.92 | 0.37 |
| N | 0.27 | 0.24 | 0.23 |
| Hydrocarbon composition, m% | |||
| Stable hydrocarbon | 29.9 | 36.7 | 36.7 |
| Aromatic hydrocarbons | 52.7 | 53.4 | 53.4 |
| Colloid | 12.6 | 9.9 | 9.9 |
| Bituminous matter | 4.8 | ＜0.1 | ＜0.1 |
| Boiling range, ℃ | |||
| Initial boiling point | 276 | 358 | 335 |
| 5％ | 387 | 405 | 390 |
| 10％ | 427 | 424 | 418 |
| 30％ | 446 | 443 | 436 |
| 50％ | 463 | 456 | 447 |
| 70％ | 477 | 467 | 460 |
| 90％ | 499 | 478 | 472 |
| 95％ | 525 | 485 | 483 |
Table 2, catalysis clarified oil underpressure distillation material distribute
| Underpressure distillation | Yield, w% |
| Distilled oil (ideal composition) | 80.2 |
| Vacuum 1st side cut (lightweight undesirable components) | 2.3 |
| Irreducible oil (the imperfect cut of heavy) | 17.5 |
| Amount to | 100.0 |
Table 3, needle-shape coke raw material require index
| Project | Index |
| Density (20 ℃), g/cm 3 | ≮1.03 |
| Ash content, ppm | ≯100 |
| Aromatic hydrocarbons, m% | ≮45 |
| Bituminous matter, m% | ≯1 |
| Sulphur content, m% | ≯0.5 |
Claims (7)
1, a kind of preprocessing method of raw materials of producing needle coke is characterized in that stock oil removes wherein undesirable components through underpressure distillation earlier, and remaining ideal composition contacts with hydrogen, hydrogenation catalyst, and the hydrogenation reaction logistics obtains producing the raw material of needle coke through separation.
2,, it is characterized in that described stock oil is selected from one or more in heavy distillate, catalytically cracked oil or clarified oil, steam cracking residual oil, the thermal cracking residue according to the method for claim 1.
3, according to the method for claim 1, it is characterized in that stock oil filtered before underpressure distillation, filtration condition is pressure 0.2～5.0MPa, 40～350 ℃ of temperature.
4,, it is characterized in that the underpressure distillation operational condition is pressure 5mmHg～100mmHg, 300～450 ℃ of temperature according to the method for claim 1.
5, according to the method for claim 1, it is characterized in that described activity of hydrocatalyst component is metal, metal oxide, the metallic sulfide of VIB, VIIB, VIIIB family element, wherein the group vib element is Mo, W, and VIIB family element is Mn, and VIIIB family element is Ni, Co, Fe.
6, according to the method for claim 1, it is characterized in that the hydrogenation reaction temperature is 300～420 ℃, reaction pressure is 1.5-5.0MPa, hydrogen-oil ratio is 50～500Nm
3/ m
3, volume space velocity 0.5～5h
-1
7, according to the method for claim 1, it is characterized in that at the bottom of the decompression Tata, adding cold residual oil, the cold residue oil temperature of described mistake is 100～350 ℃.
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| CN101776547B (en) * | 2010-01-20 | 2011-06-08 | 中国科学院山西煤炭化学研究所 | Method for easily and quickly evaluating needle coke |
| CN102839006A (en) * | 2011-06-23 | 2012-12-26 | 北京三聚创洁科技发展有限公司 | Process for purifying coal tar through centrifugation method and preparing needle coke by using coal tar |
| CN103013567A (en) * | 2011-09-28 | 2013-04-03 | 中国石油化工股份有限公司 | Method for preparing needle coke material by catalytic cracking slurry |
| CN103497779A (en) * | 2013-08-15 | 2014-01-08 | 中国石油集团东北炼化工程有限公司葫芦岛设计院 | Pretreatment method for catalytic oil slurry for needle coke production |
| CN103642511A (en) * | 2013-12-16 | 2014-03-19 | 陕西师范大学 | Preparation method of high-quality needle coke raw material |
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| CN102839006A (en) * | 2011-06-23 | 2012-12-26 | 北京三聚创洁科技发展有限公司 | Process for purifying coal tar through centrifugation method and preparing needle coke by using coal tar |
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| CN103013567A (en) * | 2011-09-28 | 2013-04-03 | 中国石油化工股份有限公司 | Method for preparing needle coke material by catalytic cracking slurry |
| CN103013567B (en) * | 2011-09-28 | 2015-02-25 | 中国石油化工股份有限公司 | Method for preparing needle coke material by catalytic cracking slurry |
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