CN101280212B - Method for processing highly acid crude oil by using delayed coking process - Google Patents
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Abstract
The invention discloses a method of machining highly-acidic crude oil through delayed coking; the method includes that highly-acidic raw material and low-acidic raw material are processed in different coking towers; the high temperature oil gas enters the same fractionating tower after the treatment; the preheated low-acidic raw material is used for leaching the coke powder in the high temperature oil gas which enters the fractionating tower and circulating the wax slop back to the low-acidic raw material coking tower. The method of machining highly-acidic crude oil through delayed coking has the advantages that the problem that the coke powder in the high temperature oil gas generated by coking during the single passing of the highly-acidic raw material cannot be eliminated through leaching in the prior art is solved; the heat energy of the fractionating tower is recovered effectively; meanwhile, the single passing operation mode is adopted by the highly-acidic crude oil coking tower to facilitate improving the processing load of the highly-acidic crude oil; besides, the wax slop can be circulated back to the low-acidic raw material coking tower for further treatment.
Description
Technical field
The invention belongs to a kind of thermo-cracking deacidifying process, specifically, is to adopt delay coking process to remove the acidic cpd in the high-acid crude oil, simultaneously high-acid crude oil is converted into a kind of method of light ends oil.
Background technology
The concentration of acid or content use total acid value to represent in the oil.With the milligram number of 1 gram crude oil or the needed Pottasium Hydroxide of all acidic components of petroleum fractions (KOH), unit was mg KOH/g during total acid value (TAN) was meant.The acid compounds that contains in the oil mainly is that the form with naphthenic acid exists, and naphthenic acid is prone to iron or the iron sulphide reaction with refining equipment, causes the corrosion of refining equipments such as tower, process furnace, pipeline, interchanger.It is generally acknowledged that the total acid value in the oil surpasses 1mg KOH/g, acid corrosion will be quite serious.
Naphthenic acid in the oil is difficult to decompose at low temperatures; Generally slower at decomposition rate below 350 ℃; Decomposition rate is just accelerated rapidly more than 380～400 ℃; Therefore can not the naphthenic acid in the oil be removed through atmospheric and vacuum distillation, not only contain higher acidic substance in the distillate behind the atmospheric and vacuum distillation, and the acid number of long residuum and vacuum residuum also can be very high.Processing crude oil with high acid value not only causes heavy corrosion to crude oil unit like this, and also can cause heavy corrosion to the following process device.Therefore, the refinery does not generally use conventional atmospheric and vacuum distillation unit processing crude oil with high acid value, need at first carry out depickling and handle.
The pyrolysis deacidifying process is exactly the principle depickling that utilizes the petroleum acid Pintsch process, all is at first high-acid crude oil to be heated to get into after 345 ℃-400 ℃ to carry out the depickling reaction in the reactor drum like the method for the processing high-acid crude oil introduced among US5976360, the US6086751.In addition, the pyrolysis deacidifying process also can add catalyzer and be beneficial to the depickling reaction, like US5928502, US5871636.The catalyse pyrolysis deacidifying process is not owing to there is good catalyzer to make acid removal rate lower at present, and deacidification effect is poor.
Delayed coking is a kind of heat processing technique that heavy oil or residual oil raw material is converted into gas, gasoline, diesel oil, wax oil cut and coke through degree of depth thermally splitting.Conventional delay coking process be with raw oil after the coking heater convection zone is preheating to 300～350 ℃; Get into coking fractional distillation column and high-temperature oil gas heat exchange from coke drum; The coke powder of carrying secretly in the high-temperature oil gas of drip washing simultaneously; Get into the coking heater radiation section after temperature is raised to 360～380 ℃ and further be heated to 480～510 ℃, get into coke drum then and carry out pyrogenic reaction.Coking oil gas flows into separation column from the coke cat head and fractionates out gas, gasoline, diesel oil, wax oil cut, and coking recycle oil gets into the process furnace radiation section with coking raw material and recycles, and sedimentation of coke is in coke drum.
CN1814704A introduces a kind of method of utilizing delay coking process to handle high-acid crude oil.This method is for fear of the acid corrosion separation column, and high-acid crude oil does not advance separation column and high-temperature oil gas heat exchange, carries out pyrolytic reaction but get in the coking tower after directly getting into process furnace and being heated to 480 ℃-510 ℃; Carry a large amount of coke powders in the high-temperature oil gas that generates, owing to there is not the drip washing of raw oil, coke powder can get into the middle and upper part of separation column with high-temperature oil gas; Cause coking in the separation column; Shorten the separation column on-stream time, and coke powder too high levels in the wax tailings, influence the quality of wax tailings.
CN1580193A introduces a kind of delayed coking method of high acid value hydrocarbon ils.This method is to get into after at first high-acid crude oil directly gets into process furnace and is heated to 350 ℃-450 ℃ to relax the cracking case internal reaction; Remove acidic components; The low sour heavy cracking thing that will generate then gets into to get in the coking tower after the process furnace radiation section is heated to 480 ℃-510 ℃ and carries out pyrolytic reaction, carries a large amount of coke powders in the high-temperature oil gas of generation secretly, directly gets into the middle and upper part of separation column owing to there is not the drip washing of raw oil; Cause coking in the separation column; Shorten the separation column on-stream time, and coke powder too high levels in the wax tailings, influence the quality of wax tailings.
Summary of the invention
To the deficiency of prior art, the invention provides a kind of delayed coking method that installs the processing high-acid crude oil that running period is long, acid removal rate is high.
Delayed coking method of the present invention adopts all the people present's coking tower (two high-acid crude oil coking towers and two low acid starting material coking towers), two process furnace (a high-acid crude oil process furnace and a low acid starting material process furnace) and a shared separation column, comprises that step is following:
(1) high-acid crude oil gets into the high-acid crude oil process furnace and is heated to 450 ℃-510 ℃; Get into then and carry out heat scission reaction in the high-acid crude oil coking tower; The high-temperature oil gas that generates is discharged from the coking cat head, gets into separation column by the separation column bottom, and the sedimentation of coke of generation is in the high-acid crude oil coking tower;
(2) get into separation column bottom and high-temperature-coked oil gas countercurrent flow, the coke powder that carries in the while drip washing coking oil gas through the low sour coking raw material of preheating from step (1) and step (3);
(3) extract out from the separation column bottom through the low sour coking raw material of heat exchange; After the low acid starting material process furnace of entering is heated to 480 ℃-510 ℃; Get into low acid starting material coking tower, under the delay coking process operational condition, carry out cracking reaction; The high-temperature oil gas that generates is discharged by the separation column bottom from the coking cat head and is got into separation column, and the sedimentation of coke of generation is in low acid starting material coking tower;
(4) in high-acid crude oil coking tower or low acid starting material coking tower, after the coke at the bottom of being deposited on coking tower is full of coking tower, stop charging, switch another coking tower and continue charging.
In the inventive method; Adopt low acid starting material to get into separation column and carry out heat exchange with high-temperature-coked oil gas from high-acid crude oil coking tower and low acid starting material coking tower; And drip washing the coke powder that carries of coking oil gas, prevented the separation column coking effectively, prolonged the separation column on-stream time; And can effectively reduce coke powder content in the wax tailings, improve the wax tailings quality.
Described high-acid crude oil was heated to before 450 ℃-510 ℃ getting into process furnace, preferably carry out heat exchange to 180 ℃-220 ℃ earlier after, and then get into the process furnace heating, effectively utilize separation column sideline product heat energy.
In the inventive method, described high-acid crude oil delayed coker operation condition is following: 450 ℃-510 ℃ of furnace outlet temperature are preferably in 470-480 ℃; Reaction pressure (absolute pressure) 0.05MPa-0.80MPa is preferably in 0.10MPa-0.18MPa; Adopt the one way pass-through mode; Residence time 10min-60min, preferably 10min-30min.
In the inventive method, the low acid starting material delayed coker operation condition of described routine is following: 450 ℃-550 ℃ of furnace outlet temperature are preferably in 495 ℃-505 ℃; Reaction pressure (absolute pressure) 0.05MPa-0.80MPa is preferably in 0.10MPa-0.18MPa; Adopt the cyclical operation mode, circulation weight ratio 0.10-1.50, preferably 0.35-1.00; Residence time 5min-60min, preferably 10min-30min.
In the inventive method, but handle each coking tower operate continuously 24 hours of conventional low acid starting material, but handle each coking tower operate continuously 48 hours of high acid starting material.
The low sour coking raw material of the routine that the present invention uses can be weight, the residual oil raw material of over point＞350 ℃; Generally can be selected from residual oil, visbroken resids, the heavy deasphalted oil of deasphalting unit, catalytically cracked oil, viscous crude, the topped crude of atmospheric and vacuum distillation unit, also can be selected from other certainly like coal processing, shale, oil-sand etc.The total acid value of low sour coking raw material is preferably less than 0.5KOHmg/g less than 1.0KOHmg/g.
Described high-acid crude oil is crude oil or the topped crude of total acid value greater than 1.0KOHmg/g.
The present invention and existing depickling compared with techniques have following advantage:
1 with the CN1814704A ratio; After high-temperature-coked oil gas got into separation column, with the raw material heat exchange of low acid starting material coking tower processing, and the coke powder that generation oil gas carries was removed in drip washing; Prevent the separation column coking; Prolong the separation column on-stream time, and can effectively reduce coke powder content in the wax tailings, improve the wax tailings quality.
2 with the CN1580193A ratio, directly get in the coking tower after high-acid crude oil directly gets into process furnace and is heated to 480 ℃-510 ℃ and carry out cracking reaction, do not need to establish again a cracking case and come first depickling, shorten flow process, reduce cost of investment and process cost.And, after high-temperature-coked oil gas gets into separation column, with the raw material heat exchange of low acid starting material coking tower processing; And drip washing removes and generates the coke powder that oil gas carries, and prevents the separation column coking, prolongs the separation column on-stream time; And can effectively reduce coke powder content in the wax tailings, improve the wax tailings quality.
The high-acid crude oil technical process adopts one way to pass through operating method in 3 the inventive method; The heavy oil that generates is handled together being recycled in the conventional coking tower with conventional raw material at the bottom of the separation column; Its advantage is to strengthen the treatment capacity of high-acid crude oil, and corrosion is limited in the cover coking tower.
The high-acid crude oil Outlet Temperature in Delayed Coking Furnace is hanged down in 4 the inventive method has following benefit:
(1) owing to contain the light constituent of the 20wt% that has an appointment in the high-acid crude oil, avoids under higher temperature of reaction, excessive fragmentation taking place, cause the generation of a large amount of gases and coke.
(2) can avoid impurity such as salt, calcium in the high-acid crude oil to be deposited on that coking results in blockage on the process furnace tube wall, prolong process furnace running period.
(3) the coking tower interior reaction temperature is relatively low, and transformation efficiency is low, and the green coke amount descends, and can prolong coking tower running period, stable operation.Save warm tower expense.
(4) save the energy.Needed oil fuel in the conservation heat-processed.
5 the inventive method turndown ratiies are big, flexibly, be easy to grasp, can be widely used.
6 the present invention can make the naphthenic acid carboxyl in the high-acid crude oil be transformed into CO, CO
2And H
2O, alkyl is transformed into hydrocarbons, thereby reaches the purpose of depickling, can effectively avoid the following process corrosion on Equipment.The acid removal rate of the inventive method reaches more than 99%.
Description of drawings
Fig. 1 is the schematic flow sheet of the inventive method.
Embodiment
Below in conjunction with Fig. 1 and the concrete further illustrated in detail of embodiment, but the present invention does not receive the restriction of embodiment.
As shown in Figure 1, high-acid crude oil gets into to get in the coking tower 5 after process furnace 3 is heated to 470 ℃-480 ℃ through pipeline 1 and reacts, and generates oil gas and gets into separating prod in the separation column 8 through pipeline 7.The coke powder that the low sour coking raw material of routine carries through heat exchange and drip washing high-temperature-coked oil gas in the convection zone heating back entering separation column 8 of pipeline 2 entering process furnace 4 after heat exchange; Get into coking tower 6 after the radiation section that gets into process furnace 4 through pipeline 9 at the bottom of the separation column then is heated to 480 ℃-510 ℃ and react, the oil gas of generation gets into separating prod in the separation columns 8 through pipeline 7.Coke goes out device through pipeline 10.After coking tower 5 and 6 is full of, stop charging, switch another coking tower 5a and 6a and carry out same operation.High-temperature oil gas from coking tower 5 and coking tower 6 is told gas 11, gasoline 12, diesel oil 13 and wax oil 14 in separation column.
High-acid crude oil among the embodiment directly gets into process furnace heating, and heater outlet temperature is 470 ℃-480 ℃, and the operational condition of coking tower is following: working pressure is that 0.12MPa-0.18MPa, reaction times 10min-30min, recycle ratio are 0.Total feed is 2kg/h, turns round 10 hours, stops charging, and adustion 2 hours is removed volatile matter.Get into separation column after the conventional coking raw material heat exchange and generate the oil gas heat exchange; Get into after getting into the process furnace radiation section then and being heated to 495 ℃-505 ℃ in the low acid starting material coking tower and react, operational condition is following: pressure is that 0.12MPa-0.18MPa, reaction times 10min-30min, recycle ratio are 0.35-1.00.Total feed is 2kg/h, turns round 10 hours, stops charging, and adustion 2 hours is removed volatile matter.
Embodiment 1-5:
Embodiment explanation: the deacidification effect of method provided by the present invention.
The method of calculation of acid removal rate are following: total acid value * 100% of acid removal rate=(total acid value of the total acid value of high-acid crude oil raw material-gained liquid-phase product)/high-acid crude oil raw material.
All experiments are identical with raw oil among the embodiment, are intended to the deacidification effect under the comparison different operating condition.
Testing used high-acid crude oil is Liaohe River viscous crude, low acid starting material xinjiang viscous crude oil, and its character is seen table 1, experiment condition and test-results are seen table 2.
The raw oil character that table 1 embodiment adopts
| Project | Liaohe River viscous crude | Xinjiang viscous crude oil |
| Density (20 ℃), kg/m 3 | 976.9 | 961.1 |
| Acid number, mgKOH/g | 8.99 | 0.05 |
| Viscosity (80 ℃), mm 2/s | 1410 | 1150 |
| Nitrogen, wt% | 0.71 | 0.53 |
| Sulphur, wt% | 0.45 | 0.18 |
| Colloid, wt% | 28.76 | 22.31 |
| Bituminous matter, wt% | 1.34 | 0.50 |
| Carbon residue, wt% | 14.57 | 10.1 |
| Vanadium, μ g/g | 2.53 | 0.67 |
| Nickel, μ g/g | 132.9 | 21.6 |
| ＜350 ℃ of yields, wt% | 9.1 | 0.0 |
| 350～500 ℃ of yields, wt% | 24.7 | 0.00 |
| ＞500 ℃ of yields, wt% | 65.1 | 100.00 |
Table 2 main technique condition and product distribute and main products character
| |
1 | 2 | 3 | 4 | 5 |
| The main operational condition of high-acid crude oil coking tower | |||||
| The furnace outlet temperature, ℃ | 480 | 470 | 475 | 475 | 480 |
| The high-acid crude oil preheating temperature, ℃ | 200 | 210 | 220 | 180 | 190 |
| Coking tower pressure, MPa | 0.18 | 0.14 | 0.16 | 0.15 | 0.12 |
| The residence time, min | 25 | 20 | 10 | 30 | 30 |
| Recycle ratio, wt | 0.0 | 0.0 | 0.0 | 0.0 | 0.0 |
| The low main operational condition of acid starting material coking tower | |||||
| The furnace outlet temperature, ℃ | 500 | 495 | 500 | 500 | 505 |
| Coking tower pressure, MPa | 0.18 | 0.14 | 0.16 | 0.15 | 0.12 |
| The residence time, |
10 | 20 | 15 | 25 | 30 |
| Recycle ratio, wt | 0.35 | 1.0 | 0.80 | 0.60 | 0.5 |
| Product distributes, wt% | |||||
| Gas | 7.5 | 7.2 | 6.9 | 8.5 | 9.2 |
| C 5 +Liquid | 72.7 | 73.3 | 74.0 | 70.6 | 69.6 |
| Coke | 19.8 | 19.5 | 19.1 | 20.9 | 21.2 |
| The liquid product total acid value, mgKOH/g | 0.01 | 0.01 | 0.01 | 0.01 | 0.01 |
| Total acid removal rate, % | ＞99 | ＞99 | ＞99 | ＞99 | ＞99 |
Claims (7)
1. the method for a delayed coking processing highly acid crude oil adopts two high-acid crude oil coking towers, two low acid starting material coking towers, a high-acid crude oil process furnace, a low acid starting material process furnace and a shared separation column, comprises that step is following:
(1) high-acid crude oil gets into the high-acid crude oil process furnace and is heated to 450 ℃-510 ℃; Get into then and carry out heat scission reaction in the high-acid crude oil coking tower; The high-temperature oil gas that generates is discharged from the coking cat head; Get into separation column by the separation column bottom and carry out fractionation, the sedimentation of coke of generation is in the high-acid crude oil coking tower, and described high-acid crude oil is the crude oil of total acid value greater than 1.0KOHmg/g;
(2) get into separation column bottom and high-temperature-coked oil gas countercurrent flow through the low sour coking raw material of preheating from step (1) and step (3); The coke powder that carries in the drip washing coking oil gas simultaneously, described low sour coking raw material are over point＞350 ℃, total acid value weight, the residual oil raw materials less than 0.5KOHmg/g;
(3) extract out from the separation column bottom through the low sour coking raw material of heat exchange; After the low acid starting material process furnace of entering is heated to 480 ℃-510 ℃, get into low acid starting material coking tower, under the delay coking process operational condition; Carry out cracking reaction; The high-temperature oil gas that generates is discharged from the coking cat head, gets into separation column by the separation column bottom and carries out fractionation, and the sedimentation of coke of generation is in low acid starting material coking tower;
(4) in high-acid crude oil coking tower or low acid starting material coking tower, after the coke at the bottom of being deposited on coking tower is full of coking tower, stop charging, switch another coking tower and continue charging.
2. according to the described method of claim 1, it is characterized in that the operational condition of described high-acid crude oil coking tower is following: 450 ℃-510 ℃ of high-acid crude oil furnace outlet temperature; Reaction absolute pressure 0.05MPa-0.80MPa; Adopt one way to pass through operating method; Residence time 10min-60min.
3. according to the described method of claim 1, it is characterized in that the operational condition of described high-acid crude oil coking tower is following: 470 ℃-480 ℃ of high-acid crude oil furnace outlet temperature; Reaction absolute pressure 0.10MPa-0.18MPa; Adopt one way to pass through operating method; Residence time 10min-30min.
4. according to the described method of claim 1, it is characterized in that the operational condition of described low acid starting material coking tower is following: 480 ℃-510 ℃ of low acid starting material furnace outlet temperature; Reaction absolute pressure 0.05MPa-0.80MPa; Adopt the cyclical operation mode, circulation weight ratio 0.10-1.5; Residence time 5min-60min.
5. according to the described method of claim 1, it is characterized in that the operational condition of described low acid starting material coking tower is following: 495 ℃-505 ℃ of low acid starting material furnace outlet temperature; Reaction absolute pressure 0.10MPa-0.18MPa; Adopt the cyclical operation mode, circulation weight ratio 0.35-1.00; Residence time 10min-30min.
6. according to the described method of claim 1, it is characterized in that described high-acid crude oil was heated to before 470 ℃-480 ℃ getting into process furnace, carry out heat exchange to 180 ℃-220 ℃ earlier.
7. according to the described method of claim 1, it is characterized in that described low sour coking raw material is selected from one or more in heavy deasphalted oil, catalytically cracked oil, viscous crude, topped crude, liquefied coal coil and the shale oil of the residual oil of atmospheric and vacuum distillation unit, visbroken resids, deasphalting unit.
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Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101724429B (en) * | 2008-10-28 | 2012-11-21 | 中国石油化工股份有限公司 | Delayed coking method for processing high-acid crude oil |
| CN102041013B (en) * | 2009-10-16 | 2013-07-24 | 中国石油化工股份有限公司 | Method for producing needle coke raw material by using delayed coking process |
| CN102051225B (en) * | 2009-10-27 | 2014-01-22 | 中国石油化工股份有限公司 | Kettle coking-hydrotreating combined process method |
| CN102268287B (en) * | 2010-06-02 | 2013-10-02 | 中国石油化工集团公司 | Delayed coking method of advanced deacidification of high acid raw oil |
| CN102268289B (en) * | 2010-06-02 | 2013-10-02 | 中国石油化工集团公司 | Delayed coking method of raw oil containing acid |
| CN102268288A (en) * | 2010-06-02 | 2011-12-07 | 中国石油化工集团公司 | Delayed coking process for deep deacidification of high-acid raw oil |
| CN102899077A (en) * | 2011-07-27 | 2013-01-30 | 中国石油化工股份有限公司 | Coking method |
| CN102504864B (en) * | 2011-10-26 | 2014-12-17 | 中国石油化工股份有限公司 | Novel process for treating thrown oil of coking towers and device thereof |
| CN104073275A (en) * | 2013-03-29 | 2014-10-01 | 广州市昊晟工程勘察设计有限公司 | Mild-reaction oil residue separation method for coal-based residual oil |
| CN104099128B (en) * | 2013-04-03 | 2015-08-19 | 中国石油天然气股份有限公司 | Method for mixed hydrogenation conversion of acid-containing petroleum and coker gas oil |
| CN103980934B (en) * | 2014-05-19 | 2015-07-01 | 华东理工大学 | Deep dehydrating method and device for oil product |
| JP7311508B2 (en) * | 2017-11-14 | 2023-07-19 | 中国石油化工股▲ふん▼有限公司 | Coking system and coking method |
| CN113092336A (en) * | 2021-04-06 | 2021-07-09 | 西南石油大学 | Device and method for researching influence of coke deposition on reservoir physical properties |
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| CN1465657A (en) * | 2002-06-27 | 2004-01-07 | 中国石油化工股份有限公司 | Method for reducing acid value of petroleum |
| CN1580193A (en) * | 2003-07-31 | 2005-02-16 | 中国石油化工股份有限公司 | High acid value hydrocarbon oil delayed coking method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1465657A (en) * | 2002-06-27 | 2004-01-07 | 中国石油化工股份有限公司 | Method for reducing acid value of petroleum |
| CN1580193A (en) * | 2003-07-31 | 2005-02-16 | 中国石油化工股份有限公司 | High acid value hydrocarbon oil delayed coking method |
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