CN1990830B - hydrorefining method for coker gasoline - Google Patents
hydrorefining method for coker gasoline Download PDFInfo
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- CN1990830B CN1990830B CN2005101355609A CN200510135560A CN1990830B CN 1990830 B CN1990830 B CN 1990830B CN 2005101355609 A CN2005101355609 A CN 2005101355609A CN 200510135560 A CN200510135560 A CN 200510135560A CN 1990830 B CN1990830 B CN 1990830B
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Abstract
The invention disclses a method of refining coking gasoline by hydrogenation, comprising following steps: mixing raw oil with hydrogen gas, feeding them into hydrogenation protection reactor for contactness with hydrogenation protecting agent and reaction at low temperature; heating the flowout product with heating furnance; feeding it into main hydrogenation reactor for contactness with hydrogenation refinery catalyst at high temperature; cooling and separating reaction product and getting hydrogen gas and refined gasoline fraction. The olefin concentration in refined gasoline fraction is lower than 1% by volume proportion, sulfur concentration is lower than 300 ug/ g, nitrogen concentration is lower than 2 ug/ g, which can meet the demand for improving pre-hydrgenation device and steam cracking olefin- preparation device. The invention is characterized in that it can effectively delay the coking speed of furnance pipe in heating furnance, largely reduce pressure- reduction generation frequency and increase the operational difficulty for main hydrogenation reactor.
Description
Technical field
The invention belongs in the method that has refining hydrocarbon ils under the situation of hydrogen, more particularly, is a kind of hydrofinishing process of coker gasoline.
Background technology
The delayed coking technology is one of important heavy oil deep processing means of China, in the product of delayed coking, (the bromine valency is 60～80gBr/100g) to coker gasoline cut olefin(e) centent height, and stability difference and octane value low (general RON＜60) should not be as the mediation components of gasoline.The processing mode of coker gasoline has four kinds at present: (1) coker gasoline is mixed to refine in the diesel hydrotreating unit and is processed, and after diesel oil hydrofining, fractionates out the hydrogenation coker gasoline; (2) coker gasoline and straight-run spirit mixed hydrogenation are refining; (3) after the full cut of coking is concentrated hydrotreatment, fractionate out the hydrogenation coker gasoline; (4) the independent hydrofining of coker gasoline.Usually with the raw material of the coker gasoline after the hydrofining, the part refinery is also arranged because the reformer insufficient raw material is incorporated into the hydrogenation coker gasoline in the reformed pre-hydrogenated device raw material as the preparing ethylene by steam cracking device.
Because coker gasoline character instability, in the course of processing, exist some problems, the independent hydrogenation mode of coker gasoline especially, the problem of existence is more outstanding.In the independent course of processing of coker gasoline, the problem of existence mainly contains two aspects: (1) reactor head coking is serious, and pressure drop is risen too fast, and most devices just needed to stop work in three months, once cast aside head to reactor; When (2) coker gasoline is through boiler tube, all vaporizations, existent gum that it is entrained and coke powder then can be attached on the boiler tube inwalls, and further decomposes becomes burnt shape thing, causes tube coking, if tube coking is serious, also can produce pressure drop.Reactor or boiler tube frequently produce pressure drop, have brought very big trouble for the production of coker gasoline hydrogenation unit.
US6090270 discloses a kind of method of handling pyrolysis gasoline, has five catalytic distillation reactors in this method at least, all feeds hydrogen stream in each catalytic distillation reactor.Stock oil with at first enter first catalytic distillation reactor, C in the stock oil after hydrogen mixes
5And C
5Behind the beds on following component contact reactor top, acetylene wherein or diolefine are removed by hydrogenation is saturated; C in the stock oil
6 +Component then enters second distillation reactor, the 3rd distillation reactor and the 4th distillation reactor successively after the first catalytic distillation reactor bottom is extracted out, wherein the C that is extracted out by the after-fractionating reactor bottom
7 +Component or C
9 +Component enters the 5th distillation reactor and further handles.This method can obtain products such as benzene,toluene,xylene and heavy naphtha, but this method flow complexity, operation easier height, and investment cost and process cost height.
US4097369 discloses a kind of treatment process of pyrolysis gasoline, this method can be handled the petroleum naphtha that is rich in olefin component, under the certain reaction condition, contacts special catalyzer and carries out aromatization, obtain being rich in the product of aromatic hydrocarbons, after fractionation, obtain benzene,toluene,xylene and C
9 +Aromatic hydrocarbons.Preferred catalyzer contains ZSM-5 zeolite, zinc and palladium.But this method also is not suitable for this diene content height of coker gasoline, inferior patrol cut that gum level is also high.
CN1035755C discloses a kind of Rifining method for catalylic cracking gasoline by adding hydrogen, this method is the prevulcanized type non-precious metal catalyst series connection that has different activities and variable grain diameter with two, segmentation is seated in the reactor or is divided in two reactors, and the circulation of a hydrofined oil part is as raw material.The maleic value of hydrogenated products is less than 1gI
2/ 100g, inductive phase was above 480 minutes.But this method also is not suitable for this diene content height of coker gasoline, inferior patrol cut that gum level is also high.
Summary of the invention
The objective of the invention is to provide on the basis of existing technology a kind of hydrofinishing process of coker gasoline.
Method provided by the invention comprises: enter the hydrogenation protecting reactor after stock oil and hydrogen mix and contact with the hydrogenation protecting agent; under the condition of 120～220 ℃ of average reaction temperature, react; its reaction effluent enters the hydrogenation main reactor after process furnace heats up; under the condition of 240～380 ℃ of average reaction temperature with the Hydrobon catalyst contact reacts; its resultant of reaction after cooling, separating, obtain hydrogen-rich gas and refining after gasoline fraction.
Present method can be handled the coker gasoline of the high nitrogen of high-sulfur, olefin(e) centent is less than 1 volume % in the gasoline fraction after refining, sulphur content is less than 300 μ g/g, and nitrogen content all can satisfy the charging requirement of reformed pre-hydrogenated device and preparing ethylene by steam cracking device less than 2 μ g/g.Present method can delay heating furnace tube coking speed effectively, reduces the pressure drop of hydrogenation main reactor greatly and produces frequency, and can improve the operating severity of hydrogenation main reactor.
Description of drawings
Accompanying drawing is the hydrofinishing process schematic flow sheet of coker gasoline provided by the invention.
Embodiment
Method provided by the invention is so concrete enforcement:
Stock oil with enter guard reactor after hydrogen mixes, at 120～220 ℃ of average reaction temperature, hydrogen dividing potential drop 1.0～8.0MPa, volume space velocity 2.0～10.0h
-1, hydrogen to oil volume ratio 100～800Nm
3/ m
3Condition under with hydrogenation protecting agent contact reacts, main under relatively low temperature, remove diolefine, glial component and metal impurities in the stock oil.The reaction effluent of hydrogenation protecting reactor enters the hydrogenation main reactor after process furnace heats up, at 240～380 ℃ of average reaction temperature, hydrogen dividing potential drop 1.0～8.0MPa, volume space velocity 1.0～6.0h
-1, hydrogen to oil volume ratio 100～800Nm
3/ m
3Condition under contact with Hydrobon catalyst, carry out that alkene is saturated, reaction such as hydrogenating desulfurization and hydrodenitrification.The resultant of reaction of hydrogenation main reactor after cooling, separating, obtain hydrogen-rich gas and refining after gasoline fraction.
Described stock oil is coker gasoline, diene content height not only in the coker gasoline, and also foreign matter content such as sulphur, nitrogen and gum level are all high, are a kind of gasoline fractions of poor quality.Present method also can be processed the high inferior patrol cut of high pressure gasoline of diene content or catalytic cracking gasoline and other foreign matter content.
Described hydrogenation protecting agent comprises hydrogenation protecting agent I and hydrogenation protecting agent II, takes top filling hydrogenation protecting agent I, the combination loading mode of bottom filling hydrogenation protecting agent II, and hydrogenation protecting agent I is 1:9～9:1 with the admission space ratio of hydrogenation protecting agent II.Hydrogenation protecting agent I and hydrogenation protecting agent II are the load catalyzer, contain a kind of alumina supporter and the molybdenum and/or the tungsten that load on this alumina supporter, and nickel and/or cobalt.Gross weight with catalyzer is a benchmark, and in oxide compound, hydrogenation protecting agent I consists of: the content of molybdenum and/or tungsten is 1～5 heavy %, and the content of nickel and/or cobalt is 0.1～2 heavy %; Hydrogenation protecting agent II consists of 3～10 heavy %, and the content of nickel and/or cobalt is 0.5～3 heavy %.Described aluminum oxide is a gama-alumina.Hydrogenation protecting agent I and hydrogenation protecting agent II have following pore distribution: bore dia be the pore volume of 100～200 dusts account for total pore volume 50～90%; bore dia be the pore volume of 200～1000 dusts account for total pore volume 5～30%; bore dia accounts for 5～40% of total pore volume greater than the pore volume of 1000 dusts, and all the other pore volumes are that diameter is occupied less than the hole of 100 dusts.
Two hydrogenation protecting agent have same carrier and same reactive metal, but the reactive metal charge capacity of hydrogenation protecting agent I is less than the reactive metal charge capacity of hydrogenation protecting agent II.Two hydrogenation protecting agent all have high catalyst activity, low coke content, low pore volume rate of descent, good activity stability and high intensity.With hydrogenation protecting agent I and hydrogenation protecting agent II in active, size and be optimized grating in shape; both can delay the speed that the hydrogenation protecting reactor pressure decrease produces; again can be with impurity removals such as the diolefine in the stock oil, glial component and metallic irons; thereby avoid heating furnace tube coking and protection main reactor, prolonged the whole device operational cycle.
Described Hydrobon catalyst is a supported non-precious metal catalyst, and carrier is unformed aluminum oxide, and reactive metal is the metal component that is selected from group vib and/or group VIII.Preferred Hydrobon catalyst is a benchmark with the catalyzer, and it consists of: nickel oxide 1～5 heavy %, and Tungsten oxide 99.999 12～35 heavy %, fluorine 1～9 heavy %, surplus is an aluminum oxide.This aluminum oxide is to be composited by one or more little porous aluminum oxides and one or more macroporous aluminium oxides weight ratio according to 75:25～50:50, the pore volume of this aperture aluminum oxide median pore diameter＜80A accounts for total pore volume more than 95%, the pore volume of this macroporous aluminium oxide median pore diameter 60～600A accounts for total pore volume more than 70%, and described pore volume is measured with B E T Brunauer Emett Teller method of nitrogen adsorption at low temperature.This Hydrobon catalyst is the solid catalyst with special shape (butterfly), and granules of catalyst is the leafy shape structure of the straight leaf of strip, and its cross section is made up of four circular leaves, and the radius of two adjacent leaves wherein is R
1, two adjacent radiuses are R in addition
2, R
1R
2This catalyzer have that the particulate granularity is little, intensity is high and use in advantages such as the beds pressure drop is low.Because this catalyzer has good hydrogenating desulfurization, hydrodenitrification and alkene saturability, can remove impurity and saturated most of alkene such as sulphur in the stock oil, nitrogen effectively.
Advantage of the present invention:
1, method flow provided by the invention is simple, and flexible and convenient operation can be used in old plant modification or the new device.Because working pressure is middle pressure, catalyzer is a non-precious metal catalyst, so investment cost and process cost are all lower.
2, use method provided by the invention; operational cycle of extension fixture greatly; slow down the speed of process furnace and the coking of hydrogenation main reactor effectively, can effectively protect hydrogenation catalyst in the hydrogenation main reactor, its reactive behavior and stability are brought into play more fully.
3, present method can be handled the coker gasoline of the high nitrogen of high-sulfur, olefin(e) centent is less than 1 volume % in the gasoline fraction after refining, sulphur content is less than 300 μ g/g, and nitrogen content all can satisfy the charging requirement of reformed pre-hydrogenated device and preparing ethylene by steam cracking device less than 2 μ g/g.
Below in conjunction with accompanying drawing method provided by the present invention is further detailed.
Accompanying drawing is the hydrofinishing process schematic flow sheet of coker gasoline provided by the invention.The hydrofinishing process technical process of coker gasoline provided by the invention is described in detail as follows: from the stock oil of pipeline 1 after feedstock pump 2 boosts and is extracted out by pipeline 3; mix with recycle hydrogen from pipeline 25; mixture is after pipeline 4 enters interchanger 5 and reaction effluent heat exchange from the hydrogenation main reactor 11 of pipeline 12; enter hydrogenation protecting reactor 7 by pipeline 6 extractions; by contacting, remove diolefine, glial component and metal impurities in the raw material with hydrogenation protecting agent bed.The outlet effluent of hydrogenation protecting reactor 7 enters process furnace 9 through pipeline 8 and heats up; logistics after the heating through pipeline 10 with enter hydrogenation main reactor 11 after small amount of recycled hydrogen from pipeline 24 mixes; by contacting, remove the impurity such as alkene, sulphur and nitrogen in the raw material with the Hydrobon catalyst bed.The reaction effluent of hydrogenation main reactor 11 enters high-pressure separator 15 successively after pipeline 12, interchanger 5, pipeline 13, air-cooler 14 coolings, carry out gas-liquid separation.Isolated liquid phase stream, the gasoline fraction after promptly making with extra care is extracted out through pipeline 16; Isolated gaseous stream, promptly hydrogen-rich gas is extracted out through pipeline 17.With after new hydrogen from pipeline 18 mixes, enter circulating hydrogen compressor inlet buffer 20 through pipeline 19 from the hydrogen-rich gas of pipeline 17, hydrogen gas stream enters circulating hydrogen compressor 22 by surge tank 20 tops through pipeline 21 and boosts.Recycle hydrogen after boosting is divided into three the tunnel: the first via is mixed with stock oil from pipeline 3 through pipeline 25; The second the tunnel mixes with furnace outlet logistics from pipeline 10 through pipeline 24, as the medium of fine setting furnace outlet temperature; Third Road enters the middle part of hydrogenation main reactor 11 through pipeline 23, and the temperature as cold hydrogen is regulated beds reduces the beds overall temperature rise, slows down catalyzer deactivation rate at high temperature.
The following examples will give further instruction to present method, but therefore not limit present method.The trade names of the hydrogenation protecting agent I that uses among the embodiment are RG-10A; the trade names of hydrogenation protecting agent II are RG-10B; the trade names of Hydrobon catalyst are RN-10B, and these catalyzer are produced by Sinopec catalyzer branch office Chang Ling catalyst plant.
Embodiment
With a kind of coker gasoline is stock oil, and stock oil character is as shown in table 1, and the maleic value of stock oil is 2.9gI/100g as shown in Table 1, and existent gum is 10mg/100ml, and sulphur content is gasoline fractions of a kind of poor quality up to 6000 μ g/g.Stock oil with enter the hydrogenation protecting reactor after recycle hydrogen mixes; contact hydrogenation protecting agent I successively and hydrogenation protecting agent II reacts; wherein the admission space of hydrogenation protecting agent I and hydrogenation protecting agent II is than being 1:2; the outlet effluent of hydrogenation protecting reactor directly enters process furnace and heats up; enter the hydrogenation main reactor then; under the effect of Hydrobon catalyst, carry out hydrofining reaction; its reaction effluent enters high-pressure separator and carries out gas-liquid separation after cooling; gasoline fraction after obtaining hydrogen-rich gas and making with extra care; reaction conditions is as shown in table 2, the main character of the outlet effluent of hydrogenation protecting reactor and refining after the main character of gasoline fraction list in table 3.As can be seen from Table 3, behind the hydrogenation protecting reactor, the material such as the impurity such as diolefine, glial component and iron that are easy to generate pressure drop in the stock oil all have been removed largely, therefore can effectively prevent the generation of furnace coking and main reactor pressure drop; Sulphur content only is 13 μ g/g in the gasoline fraction after refining, and the bromine valency only is 0.1gBr/100g, and nitrogen content only is＜0.4 μ g/g, can be used as the raw material of reformed pre-hydrogenated device or preparing ethylene by steam cracking device.
Table 1
| Stock oil | |
| Density, (20 ℃) g/cm 3 | 0.7018 |
| The bromine valency, gBr/100g | 78.7 |
| Maleic value, gI/100g | 2.9 |
| Existent gum, mg/100ml | 10 |
| Sulphur, μ g/g | 6000 |
| Nitrogen, μ g/g | 120 |
| Iron, μ g/g | 0.5 |
| Boiling range (D-86), ℃ | |
| Initial boiling point | 48 |
| 50％ | 94 |
| Final boiling point | 162 |
Table 2
| Reaction conditions | The hydrogenation protecting reactor | The hydrogenation main reactor |
| The hydrogen dividing potential drop, MPa | 3.8 | 3.5 |
| Average reaction temperature, ℃ | 180 | 300 |
| Volume space velocity, h -1 | 4.0 | 2.0 |
| Hydrogen to oil volume ratio, Nm 3/m 3 | 400 | 400 |
Table 3
| Main character | The outlet effluent of hydrogenation protecting reactor | Gasoline fraction after refining |
| The bromine valency, gBr/100g | 75 | 0.1 |
| Maleic value, gI/100g | 0.5 | |
| Existent gum, mg/100ml | Do not have | Do not have |
| Sulphur, μ g/g | 5900 | 13 |
| Nitrogen, μ g/g | 115 | <0.4 |
| Iron, μ g/g | 0.2 | |
| Boiling range (D-86), ℃ | ||
| Initial boiling point | 49 | 48 |
| 50％ | 93 | 93 |
| Final boiling point | 162 | 162 |
Claims (7)
1. the hydrofinishing process of a coker gasoline; enter the hydrogenation protecting reactor after it is characterized in that stock oil and hydrogen mixing; contact hydrogenation protecting agent I and hydrogenation protecting agent II successively; under the condition of 120～220 ℃ of average reaction temperature, react; its reaction effluent enters the hydrogenation main reactor after process furnace heats up; under the condition of 240～380 ℃ of average reaction temperature with the Hydrobon catalyst contact reacts; its resultant of reaction is through cooling; after the separation; gasoline fraction after obtaining hydrogen-rich gas and making with extra care; the admission space ratio of described hydrogenation protecting agent I and hydrogenation protecting agent II is 1: 9～9: 1, and the reactive metal charge capacity of hydrogenation protecting agent I is less than the reactive metal charge capacity of hydrogenation protecting agent II.
2. according to the method for claim 1, it is characterized in that the reaction conditions of described hydrogenation protecting reactor is: hydrogen dividing potential drop 1.0～8.0MPa, volume space velocity 2.0～10.0h
-1, hydrogen to oil volume ratio 100～800Nm
3/ m
3The reaction conditions of hydrogenation main reactor is hydrogen dividing potential drop 1.0～8.0MPa, volume space velocity 1.0～6.0h
-1, hydrogen to oil volume ratio 100～800Nm
3/ m
3
3. according to the method for claim 1, it is characterized in that described hydrogenation protecting agent I contains a kind of alumina supporter and the molybdenum and/or the tungsten that load on this alumina supporter, and nickel and/or cobalt; Gross weight with hydrogenation protecting agent I is a benchmark, and in oxide compound, the content of molybdenum and/or tungsten is 1～5 heavy %, and the content of nickel and/or cobalt is 0.1～2 heavy %.
4. according to the method for claim 1, it is characterized in that described hydrogenation protecting agent II contains a kind of alumina supporter and the molybdenum and/or the tungsten that load on this alumina supporter, and nickel and/or cobalt; Gross weight with hydrogenation protecting agent II is a benchmark, and in oxide compound, the content of molybdenum and/or tungsten is 3～10 heavy %, and the content of nickel and/or cobalt is 0.5～3 heavy %.
5. according to the method for claim 1; it is characterized in that described hydrogenation protecting agent I and hydrogenation protecting agent II have following pore distribution: bore dia be the pore volume of 100～200 dusts account for total pore volume 50～90%; bore dia be the pore volume of 200～1000 dusts account for total pore volume 5～30%; bore dia accounts for 5～40% of total pore volume greater than the pore volume of 1000 dusts, and all the other pore volumes are that diameter is occupied less than the hole of 100 dusts.
6. according to the method for claim 1, it is characterized in that described Hydrobon catalyst, is benchmark with the catalyzer, and it consists of: nickel oxide 1～5 heavy %, and Tungsten oxide 99.999 12～35 heavy %, fluorine 1～9 heavy %, surplus is an aluminum oxide.
7. according to the method for claim 1 or 6, it is characterized in that described Hydrobon catalyst particle is the leafy shape structure of the straight leaf of strip, its cross section is made up of four circular leaves, and the radius of two adjacent leaves wherein is R1, two adjacent radiuses are R2, R1＞R2 in addition.
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|---|---|---|---|
| CN2005101355609A CN1990830B (en) | 2005-12-30 | 2005-12-30 | hydrorefining method for coker gasoline |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2005101355609A CN1990830B (en) | 2005-12-30 | 2005-12-30 | hydrorefining method for coker gasoline |
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| CN1990830A CN1990830A (en) | 2007-07-04 |
| CN1990830B true CN1990830B (en) | 2011-12-21 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101343566B (en) * | 2007-07-09 | 2012-08-29 | 中国石油化工股份有限公司 | Method for improving running period of hydrogenation plant for poor petroleum naphtha |
| CN101591567B (en) * | 2008-05-29 | 2012-05-30 | 中国石油化工股份有限公司 | Method for lowering olefine content in gasoline in secondary processing |
| CN101638588B (en) * | 2008-07-31 | 2012-07-25 | 中国石油化工股份有限公司 | Combined process for delayed coking and hydrotreating |
| CN101724456B (en) * | 2008-10-23 | 2013-12-25 | 中国石油化工股份有限公司 | Hydrogenation method for producing aromatics extraction raw material |
| CN111019704A (en) * | 2019-12-11 | 2020-04-17 | 宁夏泰富能源有限公司 | Hydrogenation system is used in production of finished product oil |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1351118A (en) * | 2000-10-30 | 2002-05-29 | 中国石油化工股份有限公司 | Medium-pressure hydrogenating process for removing arylhydrocarbon from diesel oil fraction |
| CN1094967C (en) * | 1999-11-04 | 2002-11-27 | 中国石油化工集团公司 | Gasoline fraction hydrogenating and modifying method |
-
2005
- 2005-12-30 CN CN2005101355609A patent/CN1990830B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1094967C (en) * | 1999-11-04 | 2002-11-27 | 中国石油化工集团公司 | Gasoline fraction hydrogenating and modifying method |
| CN1351118A (en) * | 2000-10-30 | 2002-05-29 | 中国石油化工股份有限公司 | Medium-pressure hydrogenating process for removing arylhydrocarbon from diesel oil fraction |
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