CN106609149A - Residual oil and coal tar total fraction hydrogenation method - Google Patents
Residual oil and coal tar total fraction hydrogenation method Download PDFInfo
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Abstract
The invention relates to a residual oil and coal tar total fraction hydrogenation method; residual oil, coal tar total fractions, a catalyst and auxiliary agents are mixed to prepare oil slurry; the oil slurry is preheated in the presence of hydrogen gas, then enters a slurry bed hydrogenation reactor and is subjected to hydrogenation processing and lightening reaction, and reaction products are separated to obtain gas, hydrogenated fraction oil and solid-containing tail oil; a part of the solid-containing tail oil is circulated back to the slurry bed reactor for reaction. Compared with the prior art, the method process has no need of pretreatment of the coal tar, has the advantages of simple process and high liquid yield, and provides a processing method used for improving economical efficiency for the low-added-value residual oil and coal tar.
Description
Technical field
The present invention relates to one kind is in presence of hydrogen, residual oil and full fraction of coal tar carry out lighting and refine
Method.
Background technology
In recent years, world petroleum resource worsening shortages, and the heaviness and in poor quality problem of petroleum resources
More and more substantially, corresponding residual oil quality worse and worse, is increased using difficulty.But with global Jing
The fast development of Ji, society grows with each passing day to cleaning oil-fired demand.Therefore, it is how effectively sharp
These residual oil are used, realizes that as far as possible light oil with high yield product are current refinings to meet its growing demand
The important and difficult problem that oil interface is faced.
On the other hand, as the proportion of the unconventional resource such as the fast development of Coal Chemical Industry, coal tar gradually increases
Plus.Coal tar is the accessory substance that the processes such as coal coking, destructive distillation and crushed coal pressure gasifying are produced.Coal tar
Different from residual oil, constitute more complicated, condensed-nuclei aromatics and gum level are high, containing more oxygen-containing pole
The impurity such as property material, a certain amount of unsaturated hydrocarbons, metal and coal dust.Using conventional filtration, sink
The means such as drop and centrifugation are difficult to remove these fine impurities being dispersed in coal tar.These impurity
Presence and coal tar in a large amount of condensed-nuclei aromatics can make coal tar using fixed bed hydrogenation produce lightweight
Rapid occlusion bed during fuel oil, inactivates catalyst, produces pressure drop, has a strong impact on device
Service cycle.
Residual cracking is generally divided into two big class of decarburization and hydrogenation, is to improve residual oil weight-lightening liquid yield, closely
Residual hydrogenation route is of considerable interest over year, such as residue fixed-bed hydrogenation, boiling bed hydrogenation and slurry
State bed hydroprocessing etc., wherein slurry bed hydroprocessing due to being taken seriously with extensive adaptability to raw material, but
Current subject matter is that the asphalt content of residual oil is high, easily green coke, and the formation of coke is not only reduced
Oil yield, can also be deposited on reactor, blocking reactor or subsequent pipeline, make device contracting service cycle
It is short, do not reach industrial operation requirement.
CN103540353A discloses a kind of process coal tar and the hydrogenation combination technique of residual oil, needs first
The coal tar of removing water and solid particle is divided into≤350 DEG C of light tar cut and >=350 DEG C
Heavy coal tar fraction, heavy coal tar fraction is mixed into slurry bed system with residual oil, hydrogen and catalyst
Reactor reaction, by 350-470 DEG C of hydrogenation tail oil fixed bed residual hydrogenation equipment is delivered to；≤ 350 DEG C
Light tar cut is carried out instead with residual oil and hydrogen or hydrogenation tail oil into fixed bed residual hydrogenation equipment
Should.Although the method realizes coal tar and residual oil Combined machining, but coal tar need through dehydration,
De- solid pretreatment and atmospheric and vacuum distillation, increased equipment investment and operation energy consumption.
CN103305271A discloses a kind of combined technical method of residual oil/middle coalite tar lighting,
Hydrotreating unit is entered after feedstock oil and hydrogen mixing, all products of hydrotreating are complete without isolation
Portion enters delayed coking unit, carries out heat cracking reaction, prepares high-quality burnt；Wax tailings are fully entered
Catalytic cracking unit carries out catalytic cracking reaction, and catalytic cracking unit and delayed coking unit share one
Fractionating system, the oil gas that catalytic cracking is obtained enters fractionating system.The method can be light with maximum production
Matter oil product, obtains cleaning product oil, and production high-quality is burnt；But total oil is incorporated low, and a part of oil is turned
Low value-added coke and dry gas is turned to, energy efficiency is low.
The content of the invention
For the deficiencies in the prior art, the present invention provides a kind of residual oil and full fraction of coal tar hydrogenation side
Method, the inventive method can effectively remove the impurity in coal tar and residual oil, and coal tar and residual oil are entered
Row appropriateness lighting, obtains more fluid products.
A kind of residual oil of the present invention and full fraction of coal tar method of hydrotreating, including：
(1) residual oil, full fraction of coal tar, catalyst and auxiliary agent are hybridly prepared into slurry oil, wherein, slag
The mass ratio 10 of oil and full fraction of coal tar:90～90:10, the catalyst charge, with catalyst
Metal meter, is the 0.003%～10% of residual oil and full fraction of coal tar gross mass,
(2) in presence of hydrogen preheated rear entering is carried out at hydrogenation slurry oil in slurry bed system hydrogenation reactor
Reason and lighting reaction；
(3) step (2) product is separated, and obtains gas, hydrogenation distillate and containing solid tail oil,
Gas part loops back slurry bed system, partly loops back paste state bed reactor containing solid tail oil and is reacted；It is surplus
After remaining part point is containing solid tail oil discharger, produces steam, generate electricity or hydrogen manufacturing for gasification.
Described residual oil can be one or more heavy hydrocarbons that oil-refining chemical process is obtained；Described
The heavy hydrocarbon obtained during oil-refining chemical is that reduced crude, decompression residuum, catalytic cracking are recirculated
One kind in oil, catalytic cracked oil pulp, Aromatics Extractive Project oil, visbreaker tar, coking heavy oil and fuel oil
Or it is several.
The full fraction of coal tar is not pretreated pyrolytic tar, high temperature coal-tar or middle low temperature coal
One or more miscellas in tar.The initial boiling point of full fraction of coal tar is more than 60 DEG C, and the end point of distillation is not
Limit.The full fraction of coal tar raw material is not required to the preprocessing process such as Jing dehydrations, de- solid, depitching,
Directly mix with residual oil, catalyst, auxiliary agent, into slurry bed system hydrogenation reactor.
Wherein, the mass ratio of residual oil and full fraction of coal tar is 30:70～70:30.
The catalyst is difunctional ferrum-based catalyst, including main activity is first and helps active unit, with metal
Meter, the weight ratio first with main activity is 1 to help activity first：50～65：50, wherein, main active unit be containing
Iron compound, selected from water-soluble molysite, oxides-containing iron, containing in iron sulfide, iron-bearing mineral powder
One or more, help active unit to be zinc compound, selected from water-soluble zinc salt, containing zinc oxide,
One or more in zinc-bearing mineral powder.
It is preferred that the catalyst is constituted by oxides-containing iron and containing zinc oxide, with catalyst as entirety, with
Weight metal meter, iron content is 2%～60%, and Zn content is 1%～40%, and further preferably, iron contains
Measure as 2%～55%, Zn content is 1%～35%.
It is preferred that catalyst charge in the slurry oil, is residual oil and coal tar in terms of metal in catalyst
The 0.005%～5.0% of full cut gross mass, more preferably 0.005%～2.0%.
The auxiliary agent be sulfur-containing compound, preferred Cosan, promoter addition in the slurry oil, with sulphur
Meter, sulphur is 1～2 with the molar ratio of ferrous metal in catalyst.
The paste state bed reactor type may be selected from interior circulation tubular reactor, interior forced circulation slurry bed system
Reactor or outer forced circulation paste state bed reactor.
The operating condition of the paste state bed reactor is：300～480 DEG C of temperature, 8～20MPa of pressure,
30～300min of the slurries time of staying, hydrogen/slurry volume is than 300～1500Nm3/m3.It is preferred that slurry bed system is anti-
The operating condition for answering device is：380～460 DEG C of temperature, 8～18MPa of pressure, the slurries time of staying
60～240min, hydrogen/slurry volume is than 500～1200Nm3/m3。
Step (2) product is separated, its separation method is atmospheric and vacuum distillation, solvent extraction
Or the one or more combination in pressure filtration.After separation, gas, hydrogenation distillate are obtained and containing solid
Tail oil.The initial boiling point containing solid tail oil is 350～520 DEG C, and the solid content containing solid tail oil is not higher than 30
Weight %.Part loops back paste state bed reactor containing solid tail oil, in mass, loop back containing solid tail oil
Account for the 1%～20% of residual oil and full fraction of coal tar total feed, preferably 2%～15%.
After gained hydrogenation distillate fractionation, different distillates are carried out into fixed bed hydrogenation refined unit
Hydrofining reaction.Or boiling range is suitably hydrogenated with distillate directly as catalytically cracked material.
The reaction condition of the fixed bed hydrogenation refined unit：Hydrogen dividing potential drop is 8～15MPa, and reaction temperature is
350～410 DEG C, volume space velocity is 0.2～1.0h during liquid-1, hydrogen to oil volume ratio is 200～1000.
The hydrogenation catalyst loaded in the fixed bed hydrogenation refined unit is with hydrotreating and/or adds
At least one catalyst of hydrogen cracking function, the hydrogenation catalyst contains carrier and active metallic element,
The carrier includes at least one in aluminum oxide, amorphous silica-alumina and molecular sieve, the active metal
Element includes at least one in VIB, VIIB and group VIII element.
Compared with prior art, the advantage of the inventive method is：
(1) method that the present invention is provided, realizes the common lighting and removal of impurities of residual oil and coal tar
Journey, adaptability to raw material is wide, and coal tar raw material is not required to the pretreatments such as Jing dehydrations, de- solid, depitching,
Technological process is simplified, device and running cost is reduced, and is avoided containing the more coal tar of phenol
The environmental problem that preprocessing process is produced.
(2) present invention provide method, with respect to residuum hydroconversion for, due to introducing from coal measures
The coal tar rich in aromatic hydrocarbons, the heat endurance of the higher residual oil of asphalt content can be improved, make drip
Blue or green mass-energy is stablized and slows down or suppress asphalitine to reunite, melt and grow up so that generating the reaction of coke relatively,
Simultaneously the solid impurity in catalyst and coal tar is also provided to remove residual oil and the metal in coal tar
Place, it is to avoid it is deposited on coke laydown in the reactor, be gathered into bulk and block reactor or after
Continuous pipeline, makes device more long-term operation.
(3) method that the present invention is provided, using the relatively cheap difunctional ferrum-based catalyst of price, helps
Active unit enhances the activity of main activity unit, on the basis of product liquid property is ensured, improves liquid
Body yield, economy is provided there is provided a new way for low value-added coal tar and residual oil.
Specific embodiment
With reference to embodiment, the present invention is further illustrated, but is not therefore subject to the present invention
Any restriction.
Embodiment and the raw materials used property of comparative example are listed in table 1, and using catalyst property 2 are shown in Table.
Product is distributed on the basis of full fraction of coal tar organic moiety and residual oil gross weight.
Table 1
| Analysis project | Residual oil | Coal tar |
| Density (20 DEG C)/(g/cm3) | 1.018 | 1.082 |
| Moisture/% (w) | 0.12 | 2.25 |
| Element composition/% | ||
| C | 84.82 | 86.32 |
| H | 9.95 | 9.02 |
| S | 4.6 | 0.54 |
| N | 0.35 | 0.6 |
| O | 0.28 | 3.52 |
| Four components/% | ||
| Saturated hydrocarbons | 19.5 | 8.6 |
| Aromatic hydrocarbons | 39.2 | 57.2 |
| Colloid | 23.5 | 28.6 |
| Asphalitine | 17.8 | 5.6 |
| Metal/mg/kg | ||
| Fe | 1.0 | 79 |
| Al | 3.5 | 35 |
| Ca | 2.1 | 6.9 |
| Ni | 41 | 1.3 |
| V | 97 | 0.5 |
| Boiling range (DEG C) | ||
| Initial boiling point | 472 | 101 |
| 5% | 516 | 135 |
| 10% | 554 | 214 |
| 30% | 610 | 345 |
| 50% | 653 | 401 |
| 70% | - | 435 |
| 90% | - | 512 |
| Do | - | 525 |
Table 2
| Analysis project | Catalyst A | Catalyst B |
| Heap density (20 DEG C)/(g/cm3) | 0.996 | 1.005 |
| Constituent content/% | ||
| Fe | 20 | 35 |
| Zn | 10 | 8 |
| Average grain diameter/μm | 61 | 53 |
Embodiment 1
Using the residual oil and coal tar shown in table 1, the two ratio is 30 to the present embodiment:70, catalysis used
Agent is A, and catalyst charge (being counted with Fe and Zn sum weight) is as coal tar and residual oil gross weight
0.5%, the auxiliary agent is Cosan, promoter addition in the slurry oil, sulphur and ferrous metal in catalyst
Molar ratio be 1.Preheating furnace is pumped into after above-mentioned material mixing, catalyst is carried out in the presence of hydrogen
Sulfuration, preheating furnace mixed material out is mixed into paste state bed reactor with hydrogen partial again, in hydrogen
In the presence of gas and catalyst, the weighted BMO spaces of the impurity such as demetalization and the lightweight of partial material are carried out
After changing reaction, into hot high score, gas and liquid two parts are obtained, liquid enters separator, obtains
It is hydrogenated with distillate and containing solid tail oil, the initial boiling point containing solid tail oil is 480 DEG C, and the solid content containing solid tail oil is
8 weight %, account for combined feed quality 5% loops back paste state bed reactor containing solid tail oil, and it is besides arranged.
Reaction condition and product distribution are shown in Table 3.
Embodiment 2
Using the residual oil and coal tar shown in table 1, the two ratio is 50 to the present embodiment:50, catalysis used
Agent is B, and catalyst charge (in terms of Fe and Zn sum weight) is with coal tar and residual oil gross weight
1.0%, the auxiliary agent is Cosan, promoter addition in the slurry oil, sulphur and ferrous metal in catalyst
Molar ratio be 1.2.Preheating furnace is pumped into after above-mentioned material mixing, is catalyzed in the presence of hydrogen
Agent vulcanizes, and preheating furnace mixed material out is mixed into paste state bed reactor with hydrogen partial again,
In the presence of hydrogen and catalyst, carry out the impurity such as demetalization weighted BMO spaces and partial material it is light
After matterization reaction, into hot high score, gas and liquid two parts are obtained, liquid enters separator, obtains
To hydrogenation distillate and containing solid tail oil, the initial boiling point containing solid tail oil is 400 DEG C, the solid content containing solid tail oil
For 5 weight %, account for combined feed quality 15% loops back paste state bed reactor containing solid tail oil, and it is besides
Row.Reaction condition and product distribution are shown in Table 3.
Embodiment 3
Using the residual oil and coal tar shown in table 1, the two ratio is 30 to the present embodiment:70, catalysis used
Agent is A, and catalyst charge (in terms of Fe and Zn sum weight) is with coal tar and residual oil gross weight
1.0%, the auxiliary agent is Cosan, promoter addition in the slurry oil, sulphur and ferrous metal in catalyst
Molar ratio be 1.5.Preheating furnace is pumped into after above-mentioned material mixing, is catalyzed in the presence of hydrogen
Agent vulcanizes, and preheating furnace mixed material out is mixed into paste state bed reactor with hydrogen partial again,
In the presence of hydrogen and catalyst, carry out the impurity such as demetalization weighted BMO spaces and partial material it is light
After matterization reaction, into hot high score, gas and liquid two parts are obtained, liquid enters separator, obtains
To the liquid oil (hydrogenation distillate) of different fractions section and containing solid tail oil, the initial boiling point containing solid tail oil is
510 DEG C, the solid content containing solid tail oil is 15 weight %, accounts for circulating containing solid tail oil for combined feed quality 2%
Overfall state bed reactor, remaining is containing row outside solid tail oil.Reaction condition and product distribution are shown in Table 3.
Comparative example 1
Using the residual oil and coal tar shown in table 1, the two ratio is 30 to this comparative example:70, catalysis used
Agent is iron ore, catalyst charge (in terms of Fe) with the 1.0% of coal tar and residual oil gross weight,
Preheating furnace is pumped into after above-mentioned material mixing, catalyst vulcanization is carried out in the presence of hydrogen, preheating furnace goes out
The mixed material for coming is mixed into paste state bed reactor with hydrogen partial again, in hydrogen and the work of catalyst
With under, after carrying out the weighted BMO spaces of the impurity such as demetalization and the lighting reaction of partial material, enter
Hot high score, obtains gas and liquid two parts, and liquid enters separator, obtains the liquid of different fractions section
Body oil and containing solid tail oil, arranges containing outside solid tail oil.Reaction condition and product distribution are shown in Table 3.
Comparative example 2
Using the residual oil and coal tar shown in table 1, the two ratio is 50 to this comparative example:50, by coal tar
Distilled, be divided into less than or equal to 350 DEG C and more than 350 DEG C of two parts, the two yield is respectively 30%
With 66.5%, gas recovery ratio is 3.5%, used to urge by residual oil and coal tar mixing more than 350 DEG C
Agent is iron ore, and catalyst charge (in terms of Fe) is with total coal tar and residual oil gross weight
1.0%, preheating furnace is pumped into after above-mentioned material mixing, catalyst vulcanization is carried out in the presence of hydrogen, in advance
Hot stove mixed material out is mixed into paste state bed reactor with hydrogen partial again, in hydrogen and catalysis
In the presence of agent, the weighted BMO spaces of the impurity such as demetalization and the lighting reaction of partial material are carried out,
Coking is serious in operation 24h reactors, into hot high score, obtains gas and liquid two parts, liquid
Into separator, the liquid oil of different fractions section is obtained and containing solid tail oil, arrange containing outside solid tail oil.Reaction
Condition and product distribution are shown in Table 3.
Table 3
| Project | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 |
| Reaction condition | |||||
| Temperature of reactor/DEG C | 430 | 420 | 450 | 430 | 430 |
| Reactor pressure/MPa | 18 | 20 | 18 | 18 | 18 |
| Air speed/h-1 | 1.0 | 0.5 | 1.5 | 1.0 | 1.0 |
| Catalyst | A | B | A | Iron ore | Iron ore |
| Product slates/weight % | |||||
| Gas | 7.1 | 7.5 | 6.3 | 8.4 | 7.8 |
| Gasoline fraction | 18.3 | 18.8 | 18.3 | 16.2 | 17.7 |
| Diesel oil distillate | 44.9 | 42.8 | 45.8 | 35.5 | 32.5 |
| Wax oil cut | 25.1 | 25.8 | 23.3 | 26.7 | 24.2 |
| Containing solid tail oil | 3.8 | 4.5 | 5.2 | 11.1 | 12.2 |
| Coke | 0.8 | 0.6 | 1.1 | 2.1 | 5.6 |
| Liquid oily yield/weight % | 88.3 | 86.1 | 87.4 | 78.4 | 74.4 |
Can be seen that using method of the present invention by the embodiment and comparative example in table 3, coke is received
Rate be less than 1.5%, liquid oil yield be more than 86%, compare proportional liquid oil yield it is high 9 percentage points with
On.It follows that the inventive method can improve liquid oil yield, coke yield is reduced, realize dress
Long-term operation is put, larger economic benefit is produced.
Claims (10)
1. a kind of residual oil and full fraction of coal tar method of hydrotreating, including：
(1) residual oil, full fraction of coal tar, catalyst and auxiliary agent are hybridly prepared into slurry oil, wherein, slag
The mass ratio 10 of oil and full fraction of coal tar:90～90:10, the catalyst charge, with catalyst
Metal meter, is the 0.003%～10% of residual oil and full fraction of coal tar gross mass；
(2) in presence of hydrogen preheated rear entering is carried out at hydrogenation slurry oil in slurry bed system hydrogenation reactor
Reason and lighting reaction；
(3) step (2) product is separated, and obtains gas, hydrogenation distillate and containing solid tail oil,
Gas part loops back slurry bed system, partly loops back paste state bed reactor containing solid tail oil and is reacted；It is surplus
After remaining part point is containing solid tail oil discharger, produces steam, generate electricity or hydrogen manufacturing for gasification.
2. in accordance with the method for claim 1, it is characterised in that the catalyst is difunctional iron-based
Catalyst, including main activity is first and helps active unit, in terms of metal, the weight for helping activity first with main active unit
Amount is than being 1：50～65：50, wherein, it is main activity unit be iron containing compoundses, selected from water-soluble molysite,
Oxides-containing iron, containing one or more in iron sulfide, iron-bearing mineral powder, help active unit be containing
Zinc compound, selected from water-soluble zinc salt, containing one or more in zinc oxide, zinc-bearing mineral powder.
3. according to the method described in claim 1 or 2, it is characterised in that the catalyst is by iron content oxygen
Compound and containing zinc oxide composition, with catalyst as entirety, with metal weight, iron content is
2%～60%, Zn content is 1%～40%.
4. according to the method described in claim 1 or 3, it is characterised in that catalyst adds in the slurry oil
Enter amount, be the 0.005%～5.0% of residual oil and full fraction of coal tar gross mass in terms of metal in catalyst.
5. according to the method described in Claims 2 or 3, it is characterised in that the auxiliary agent is sulfur-bearing chemical combination
Thing, promoter addition in the slurry oil, sulphur is 1～2 with the molar ratio of ferrous metal in catalyst.
6. in accordance with the method for claim 1, it is characterised in that the operation of the paste state bed reactor
Condition is：300～480 DEG C of temperature, 8～20MPa of pressure, 30～300min of the slurries time of staying, hydrogen/
Slurry volume is than 300～1500Nm3/m3。
7. in accordance with the method for claim 1, it is characterised in that step (2) product is carried out
Separate, its separation method is one or more groups in atmospheric and vacuum distillation, solvent extraction or pressure filtration
Close.
8. in accordance with the method for claim 1, it is characterised in that the initial boiling point containing solid tail oil is
350～520 DEG C, the solid content containing solid tail oil is not higher than 30 weight %.
9. according to the method described in claim 1 or 8, it is characterised in that partly loop back containing solid tail oil
Paste state bed reactor, in mass, loop back account for residual oil containing solid tail oil and full fraction of coal tar is always entered
The 1%～20% of doses, preferably 2%～15%.
10. in accordance with the method for claim 1, it is characterised in that the full fraction of coal tar is not for
One or more miscellas in pretreated pyrolytic tar, high temperature coal-tar or middle coalite tar.
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| CN116948683A (en) * | 2023-09-15 | 2023-10-27 | 克拉玛依市先能科创重油开发有限公司 | Slurry bed reaction on-line switching method using cycloalkyl residual oil and ethylene cracking tar as raw materials |
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| CN106609149B (en) | 2018-07-31 |
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