CN102051225A - Kettle coking-hydrotreating combined process method - Google Patents
Kettle coking-hydrotreating combined process method Download PDFInfo
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- CN102051225A CN102051225A CN2009101881439A CN200910188143A CN102051225A CN 102051225 A CN102051225 A CN 102051225A CN 2009101881439 A CN2009101881439 A CN 2009101881439A CN 200910188143 A CN200910188143 A CN 200910188143A CN 102051225 A CN102051225 A CN 102051225A
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Abstract
The invention discloses a kettle coking-hydrotreating combined process method, which comprises the following steps of: performing coking reaction on coking materials in a kettle coking device; introducing high temperature oil gas generated in the reaction into a coke powder removing tank filled with an inert solid filler to remove coke powder carried in the high temperature oil gas; discharging a gas phase from the top of the coke powder removing tank, and introducing into a gas-liquid separating tank for gas-liquid separation; and introducing the separated liquid and a liquid phase discharged from the bottom of the coke powder removing tank after heat exchange into a hydrogenation reactor for hydrotreating to obtain fuel oil or industrial chemicals, wherein coke generated in the coking reaction is discharged from the device and needle coke with an anisotropic optical structure is obtained. Compared with the conventional coking process, the kettle coking-hydrotreating combined process method has the advantages that: the coke yield is high through kettle coking, the quality of the needle coke is high, a coking fractional distillation tower is not needed for fractional distillation of products, the investment and operating cost are greatly reduced, and by combining the hydrotreating, the high-quality fuel oil or industrial chemicals can be obtained.
Description
Technical field
The invention belongs to coking and hydrotreater process integration technology.Specifically, be still formula coking production high-quality needle coke, liquid product enters hydrogenation unit after filtering simultaneously, and hydrogenated products are a kind of method of high-grade fuel or high-quality industrial chemicals.
Background technology
Needle coke is a raw material of producing superpower and ultra-high power graphite electrode.Superpower and ultra-high power graphite electrode are widely used in steel-making, aluminium metallurgy production and the national defense construction.The fast development of steel industry, increasing to the demand of superpower and ultra-high power graphite electrode, therefore, the demand of raw material-needle coke of producing superpower and ultra-high power graphite electrode is also increased sharply.
The most critical issue of producing needle coke is not only the selection and the pre-treatment of raw material, and the processing mode of selection and optimal operation conditions are most important to the quality of the needle coke produced.
CN1382761A discloses a kind of method of utilizing preparing acicular coke by catalytic cracking of classified oil.This method mainly is to utilize extraction process to remove catalyst fines in the fluid catalytic cracking decant oil, utilizes delay coking process to produce needle coke then.CN1944578A discloses a kind of technology of utilizing coal-tar pitch to produce needle coke.The pre-treatment of needle-shape coke raw material is through processes such as flash distillation, fractional condensation, polycondensations in this process; Adopt the fractional condensation method after the flash distillation, with the full cut of flash oil again through two sections condensation process, tell light, in, heavy constituent, flash oil light, middle component further circulated mixes with heavy constituent again after the polycondensation, as the raw material of production needle coke.Then this raw material is carried out delayed coking under the condition that nitrogen exists and handle, produce needle coke.
At present, domestic general use delayed coker produces needle coke, technology maturation.The oil gas that generates enters separation column, carries out product separation.Main products is reacted gas and gasoline fraction, diesel oil distillate, wax oil cut, and tail oil returns coking tower as turning oil.Wherein gasoline fraction, diesel oil distillate, wax oil cut can carry out hydrotreatment respectively, also can mix back end hydrogenation and handle, and obtain high-grade fuel oil or high-quality industrial chemicals.
Summary of the invention
At the deficiencies in the prior art, the invention provides a kind of still formula coking-hydrotreatment combined processing method.This method not only can improve the quality and the productive rate of needle coke, and can produce high-grade fuel oil or high-quality industrial chemicals.
Still formula coking of the present invention-hydrotreatment combined processing method, comprise that coking raw material carries out pyrogenic reaction in still formula coker, the high-temperature oil gas that reaction generates enters the decoking powder jar that inert solid fillers is housed, remove the coke powder that carries in the high-temperature oil gas, gas phase is discharged from the top of decoking powder jar, enter knockout drum and carry out gas-liquid separation, the liquid phase that separating obtained liquid and the decoking powder pot bottom after the heat exchange are discharged together enters hydrogenator and carries out hydrotreatment, obtains oil fuel or industrial chemicals; Wherein the coke of pyrogenic reaction generation goes out device, obtains the needle coke of anisotropy optics structure.
In the inventive method, described still formula coker is equipped with the built-in electrode rod, by electrode bar to the stock oil heating that heats up, under the processing condition of suitable for producing needle coke, can produce the needle coke with anisotropy optics structure, described operational condition is as follows: 300 ℃～350 ℃ of raw material heat exchange temperature; Reaction pressure 1.0MPa～2.0MPa; 400 ℃～520 ℃ of temperature of reaction; Reaction time 5h～25h.Optimum operation condition is as follows: 450 ℃～470 ℃ of temperature of reaction; Reaction pressure 1.3MPa～1.7MPa; Reaction time 16h～20h.
Still formula coking raw material of the present invention is the weight that contains aromatic hydrocarbons, the residual oil raw material of initial boiling point＞350 ℃, comprises in catalytically cracked oil, vacuum residuum, visbroken resids, furfural extract oil and the coal tar one or more.
In the inventive method, the inert solid fillers that is used for removing coke powder in the described decoking powder jar is one or more of stainless steel, pottery, coker refinery coke, inertia aluminum oxide and the inertia silicon oxide produced, and its shape can be one or more in sphere, bar shaped, annular, Raschig ring, Pall ring, cascade ring and the rectangular saddle ring.The nominal diameter of inert solid fillers is 1～20mm, preferred 2～5mm.In the methods of the invention, the nominal diameter of inert solid fillers of coking oil gas ingress filling that is preferably in described decoking powder jar is greater than the inert solid fillers in downstream, at the coking oil gas ingress of decoking powder jar filling nominal diameter is 3～25mm, the inert solid fillers of 5～12mm preferably, described ingress inert solid fillers volume accounts for 20%～40% of total filler volume, prevent that ingress coke powder concentration is big, result in blockage.
In the inventive method, the inert solid fillers bed layer pressure in decoking powder jar reaches 0.1MPa～0.2MPa, switches another decoking powder jar; The coke powder on the inert solid fillers is burnt in the decoking powder jar blowing air oxidizing fire regeneration of switching, and does not perhaps regenerate, and directly changes inert solid fillers; If solid packing is a refinery coke, preferably more change.
Hydrotreatment of the present invention can be adopted conventional hydrogenation technique and hydrotreating catalyst, described hydrotreating catalyst, be active metal component generally with group vib and/or group VIII metal, with aluminum oxide or siliceous aluminum oxide is carrier, the group vib metal is generally Mo and/or W, the group VIII metal is generally Co and/or Ni, and the active metal component in the inventive method in the used hydrotreating catalyst is preferably selected Co-Mo, Ni-Mo or Ni-W for use.In the weight of catalyzer, the group vib metal content is counted 10wt%～35wt% with oxide compound, and the group VIII metal content is counted 3wt%～15wt% with oxide compound, and its character is as follows: specific surface is 100～650m
2/ g, pore volume are 0.15～0.6ml/g.The for example FH-5 of Fushun Petrochemical Research Institute's development and production, FH-98,3936, hydrotreating catalysts such as 3996.Described hydroprocessing condition is as follows: temperature of reaction is 300 ℃～380 ℃, and reaction pressure is 4.0MPa～8.0MPa, and volume space velocity is 1.0h during liquid
-1～5.0h
-1, hydrogen to oil volume ratio is 300～800.
Characteristics of the present invention are that the cracked product of coking process production is no longer segmented from going out products such as gas, gasoline, diesel oil through coking fractional distillation column, but tell gaseous products through decoking powder jar, after the liquid-phase mixing that the liquid and the decoking powder pot bottom of gained after the gas-liquid separation comes out, directly enter hydrotreater, produce high-grade fuel oil or high-quality industrial chemicals.
The present invention compared with prior art has following advantage:
1, compare with CN1944578A technology with CN1382761A, still formula coking coking yield height, needle coke productive rate height wherein, intensity is good.Because the disposable charging of still formula coking, the amount that the gas of controlling well generates reaches unanimity the pulling force of unit time by the air-flow focusing layer of burnt layer, the coking yield height, and the needle coke productive rate of generation is also high, and quality is good.
2, decoking powder jar can remove 60%～80% with the coke powder that carries in the coking oil gas, has alleviated coking greatly and has generated oil and enter the burden that removes dust before the hydrogenation unit.
3, owing to the coking yield height, component heavier in the raw material has generated coke substantially, makes the liquid-phase product of generation lighter, and final boiling point is low, can obtain high-grade fuel oil or high-quality industrial chemicals after hydrotreatment.
4, the coking of still formula generate oil distillate gentlier, narrower, help the operation and the selection of catalysts of hydrogenation unit.
5, the inventive method technical process is short, simple to operate.
6, cost of investment and process cost have been reduced.
Description of drawings
Fig. 1 is the schematic flow sheet of the inventive method.
Embodiment
The inventive method detailed process is as follows: raw material 1 generates oil 6 with coking and enters in the still formula coking reactor 4 by pipeline 3 or 3A after the heat exchange in interchanger 12, carry out pyrogenic reaction, the coke that generates goes out device by pipeline 7, generate oil by pipeline 9 and 10 or 10A enter in the decoking powder jar 5 and carry out the decoking powder, gas phase is discharged by pipeline 11 at decoking powder jar 5 tops, enter and carry out gas-liquid separation in the drainer 20, gas goes out device by pipeline 21, separating the liquid that obtains mixes with the heavier oil product of telling from decoking powder jar 5 bottoms after heat exchange by pipeline 8, together enter hydrogenation unit 13, hydrogenated oil enters knockout tower 15 by pipeline 14 and carries out the product fractionation, obtain a small amount of gas 16, hydrogenated gasoline cut 17 and hydrogenated diesel oil cut 18, tail oil goes out device by 22.After coking still 4 is full of, switches 4A and operate equally; Decoking powder jar 5 is full of back switching 5A and carries out same operation, and decoking powder flash tank 5 filler-changeables also can be regenerated filler.
Fig. 1 is employed a kind of schematic flow sheet in following examples of the present invention.Be further explained in detail the present invention below in conjunction with accompanying drawing and specific embodiment.
The following examples will be elaborated to the inventive method, but the present invention is not subjected to the restriction of embodiment.
Among the embodiment, come from and enter in the still formula coking reactor after the needle-shape coke raw material handled well and coking generate oily heat exchange to 300 ℃～350 ℃, be heated to 450 ℃～470 ℃ of temperature of reaction by built-in electrode bar; Reaction pressure 1.3MPa～1.7MPa; Reaction time 16h～20h.The reaction later stage improves temperature of reaction and is no more than 520 ℃, and adustion 2 hours is removed volatile matter.
Embodiment 1-4
Embodiment 1 adopts conventional delay coking process, and embodiment 2～4 adopts the still formula coking-hydrogenation process integration of the inventive method.
For ease of relatively, the needle coke that conventional delay coking process is produced and product distributes and part main character (seeing embodiment 1) contrasts with the inventive method (embodiment 2～4), data are listed in the table in the lump.
All experiments use stock oil identical among the embodiment, and the coke chemicals that are intended under the different complete processings of comparison distribute and product property.
Testing raw materials used oil is catalytically cracked oil, and character sees Table 1, and experiment condition and test-results see Table 2.
Used inert solid fillers is a stupalith among the embodiment, and nominal diameter is 4mm, annular shape; The ingress inert solid fillers is a stupalith, and nominal diameter is 6mm, annular shape.Ingress inert solid fillers volume accounts for 30% of total filler volume.
The used hydrotreating catalyst of employed hydrogenation unit is the FH-98 of Fushun Petrochemical Research Institute's development among the embodiment.The hydrogenation reaction temperature is 340 ℃; Reaction pressure is 6.0MPa; Volume space velocity is 2.0h during liquid
-1Hydrogen to oil volume ratio is 500.
The stock oil character that table 1 embodiment adopts
| Raw material | The FCC slurry oil |
| Density (20 ℃)/kg/m -3 | 1.0058 |
| Viscosity (100 ℃)/mm 2·s 1 | 10.00 |
| Condensation point/℃ | 34 |
| Carbon residue, % (massfraction) | 6.10 |
| Ash content, % (massfraction) | 0.172 |
| S，％ | 0.43 |
| N/μg·g -1 | 3678 |
| C, % (massfraction) | 88.44 |
| H, % (massfraction) | 8.90 |
| Four components, % (massfraction) | |
| Saturated branch | 30.1 |
| Fragrance divides | 56.2 |
| Colloid | 13.2 |
| Bituminous matter | 0.5 |
| Metal composition/μ gg -1 | |
| Fe/Ca | 114.7/47.25 |
| Ni/V | 88.6/5.175 |
| Na | 61.79 |
Table 2 main technique condition and product distribute
| Embodiment | 1 | 2 | 3 | 4 |
| Main operational condition: | ||||
| The furnace outlet temperature, ℃ | 490 | |||
| Still formula pyrogenic reaction temperature, ℃ | 450 | 460 | 470 | |
| Pyrogenic reaction pressure, MPa | 1.7 | 1.7 | 1.6 | 1.4 |
| Reaction times, |
18 | 20 | 16 | 18 |
| Device combined feed total feed (massfraction), % | 100.0 | 100.0 | 100.0 | 100.0 |
| Product distributes (massfraction), % | ||||
| Gas | 8.2 | 15.2 | 14.9 | 15.8 |
| C5-350℃ | 29.7 | 32.5 | 30.3 | 28.8 |
| ＞350℃ | 25.5 | - | - | - |
| Coke | 36.6 | 52.3 | 54.8 | 55.4 |
Table 3 generates oil nature
Table 4 hydrogenation technique condition
| Reaction pressure, MPa | 6.0 |
| Volume space velocity during liquid, h -1 | 3.0 |
| Average reaction temperature, ℃ | 340 |
| Hydrogen to oil volume ratio | 500 |
| Hydrotreating catalyst | FH-98 |
The main character of table 5 hydrotreatment product
| Title | Hydrogenated gasoline | Hydrogenated diesel oil |
| Density (20 ℃), g/cm 3 | 0.7124 | 0.8323 |
| Boiling range, ℃ | ||
| IBP/10％ | 40/68 | 161/183 |
| 30％/50％ | 86/103 | 213/234 |
| 70％/90％ | 121/140 | 259/298 |
| EBP | 163 | -/348 |
| Sulphur, μ g/g | ＜5 | ＜20 |
| Nitrogen, μ g/g | ＜2 | ＜10 |
| Cetane value | 41 | |
| Cetane index (ASTM D 4737-96a) | 43.4 |
The main character of table 6 needle coke
Annotate: the per-cent of ash content and volatile matter is massfraction.
Claims (16)
1. still formula coking one hydrotreatment combined processing method, comprise that coking raw material carries out pyrogenic reaction in still formula coker, the high-temperature oil gas that reaction generates enters the decoking powder jar that inert solid fillers is housed, remove the coke powder that carries in the high-temperature oil gas, gas phase is discharged from the top of decoking powder jar, enter knockout drum and carry out gas-liquid separation, the liquid phase that separating obtained liquid and the decoking powder pot bottom after the heat exchange are discharged together enters hydrogenator and carries out hydrotreatment, obtains oil fuel or industrial chemicals; Wherein the coke of pyrogenic reaction generation goes out device, obtains the needle coke of anisotropy optics structure.
2. in accordance with the method for claim 1, it is characterized in that described inert solid fillers is one or more in stainless steel, pottery, coker refinery coke, inertia aluminum oxide and the inertia silicon oxide produced, its shape can be one or more in sphere, bar shaped, annular, Raschig ring, Pall ring, cascade ring and the rectangular saddle ring.
3. according to claim 1 or 2 described methods, the nominal diameter that it is characterized in that described inert solid fillers inert solid fillers is 1～20mm.
4. according to claim 1 or 2 described methods, the nominal diameter that it is characterized in that described inert solid fillers inert solid fillers is 2～5mm.
5. in accordance with the method for claim 1, it is characterized in that, the nominal diameter of the inert solid fillers of loading in the coking oil gas ingress of described decoking jar is greater than the inert solid fillers in downstream, and described ingress inert solid fillers volume accounts for 20%～40% of total filler volume.
6. in accordance with the method for claim 5, it is characterized in that the nominal diameter of the inert solid fillers of loading in the coking oil gas ingress of described decoking jar is 3～25mm.
7. in accordance with the method for claim 5, it is characterized in that, is the inert solid fillers of 5～12mm at the coking oil gas ingress of described decoking jar filling nominal diameter.
8. in accordance with the method for claim 1, it is characterized in that the inert solid fillers bed layer pressure in described decoking powder jar reaches 0.1MPa～0.2MPa, switch another decoking powder jar; Inert solid fillers is perhaps directly changed in the decoking powder jar blowing air oxidizing fire regeneration of switching.
9. in accordance with the method for claim 1, it is characterized in that described still formula coker is equipped with the built-in electrode rod, by electrode bar to the stock oil heating that heats up.
10. according to claim 1 or 9 described methods, it is characterized in that described coking operation condition is as follows: 300 ℃～350 ℃ of the temperature after the raw material heat exchange, reaction pressure 1.0MPa～2.0MPa, 400 ℃～520 ℃ of temperature of reaction, reaction time 5h～25h.
11. in accordance with the method for claim 10, it is characterized in that described coking operation condition is as follows: 450 ℃～470 ℃ of temperature of reaction, reaction pressure 1.3MPa～1.7MPa, reaction time 16h～20h.
12. in accordance with the method for claim 10, it is characterized in that described still formula coking raw material is the weight that contains aromatic hydrocarbons, the residual oil raw material of initial boiling point＞350 ℃.
13. in accordance with the method for claim 10, it is characterized in that described heavy, residual oil raw material is one or more in catalytically cracked oil, vacuum residuum, visbroken resids, furfural extract oil and the coal tar.
14. in accordance with the method for claim 1, it is characterized in that the hydrotreating catalyst that described hydrotreatment is adopted, is active metal component with group vib and/or group VIII metal, is carrier with aluminum oxide or siliceous aluminum oxide; In the weight of catalyzer, the group vib metal content is counted 10wt%～35wt% with oxide compound, and the group VIII metal content is counted 3wt%～15wt% with oxide compound, and its character is as follows: specific surface is 100～650m
2/ g, pore volume are 0.15～0.6ml/g.
15. in accordance with the method for claim 14, it is characterized in that the active metal component in the used hydrotreating catalyst selects Co-Mo, Ni-Mo or Ni-W for use.
16. according to claim 1 or 14 described methods, it is characterized in that described hydroprocessing condition is as follows: temperature of reaction is 300 ℃～380 ℃, and reaction pressure is 4.0MPa～8.0MPa, volume space velocity is 1.0h during liquid
-1～5.0h
-1, hydrogen to oil volume ratio is 300～800.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105623693A (en) * | 2014-10-31 | 2016-06-01 | 中国石油化工股份有限公司 | Method for preparing raw material for needle-like coke |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1184841A (en) * | 1997-06-18 | 1998-06-17 | 锦州石化天元集团公司 | Technology for processing tar from delayed coking process |
| CN101280212A (en) * | 2007-04-04 | 2008-10-08 | 中国石油化工股份有限公司 | Method for processing highly acid crude oil by using delayed coking process |
| CN101343567A (en) * | 2007-07-09 | 2009-01-14 | 中国石油化工股份有限公司 | Process integration for carbonization-carbonization full cut fraction hydrotreatment |
-
2009
- 2009-10-27 CN CN200910188143.9A patent/CN102051225B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1184841A (en) * | 1997-06-18 | 1998-06-17 | 锦州石化天元集团公司 | Technology for processing tar from delayed coking process |
| CN101280212A (en) * | 2007-04-04 | 2008-10-08 | 中国石油化工股份有限公司 | Method for processing highly acid crude oil by using delayed coking process |
| CN101343567A (en) * | 2007-07-09 | 2009-01-14 | 中国石油化工股份有限公司 | Process integration for carbonization-carbonization full cut fraction hydrotreatment |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105623693A (en) * | 2014-10-31 | 2016-06-01 | 中国石油化工股份有限公司 | Method for preparing raw material for needle-like coke |
| CN105623693B (en) * | 2014-10-31 | 2018-07-31 | 中国石油化工股份有限公司 | A method of preparing needle-shape coke raw material |
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