CN105733668A - Coal tar hydrogenation treatment method - Google Patents
Coal tar hydrogenation treatment method Download PDFInfo
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- CN105733668A CN105733668A CN201410732099.4A CN201410732099A CN105733668A CN 105733668 A CN105733668 A CN 105733668A CN 201410732099 A CN201410732099 A CN 201410732099A CN 105733668 A CN105733668 A CN 105733668A
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Abstract
The invention provides a coal tar hydrogenation treatment method. The method is as below: first conducting hydrogenation reaction on coal tar and hydrogen in a fluidized bed reaction zone in a hydrogenation reactor; dehydrating the reaction products and fractionating to obtain light components and heavy components; returning part of the heavy components to the fluidized bed reaction zone or throwing outside part of the heavy components; and reacting light components in a fixed bed reaction zone in the hydrogenation reactor, fractionating the reaction products to obtain gas, naphtha and diesel. The hydrogenation reactor is a concentric cylinder-shaped reactor comprising an inner cylinder and an outer cylinder; the inner cylinder is the fluidized bed reaction zone, and the outer cylinder is the fixed bed reaction zone; the fluidized bed reaction zone and the fixed bed reaction zone do not communicate with each other, and are respectively provided with an intake feed pipe and a discharge pipe. The method of the invention can effectively alleviate the temperature rising in the fluidized bed reaction zone, reduce the amount of quench oil, also can eliminate a heating furnace required for light component fixed bed reaction zone hydrogenation in the prior art, and save equipment investment.
Description
Technical field
The processing method that the present invention relates to coal tar, especially relates to a kind of hydrotreating method rich in aromatic hydrocarbons and the coal tar of colloid.
Background technology
Coal tar is the product liquid obtained in the dry distillation of coal and gasification, Coal at Normal Temperature tar is a kind of dark thick liquid, and density is higher, is mainly made up of polycyclc aromatic compound, coal tar oil composition is extremely complex, and species that are separated at present and that identify have kind more than 500.Relative petroleum refining process, coal tar obtains under the high temperature conditions, wherein contain substantial amounts of alkadienes, the unsaturated hydrocarbons such as aromatic hydrocarbon and colloid, saturated hydrocarbons and asphalt content are relatively fewer, in some coal tar, the summation of aromatic hydrocarbon and colloid can account for more than 90%, these components release substantial amounts of heat in hydroprocessing processes, cause bed temperature runaway, bed " focus " is caused to occur, according to on-the-spot actual industrial working order reflection, temperature rise can reach more than 100 DEG C, for avoiding the high temperature rise impact on catalyst performance, real-world operation process needs carry out noting cold hydrogen or note quench oil operation to reduce temperature rise, this operation unavoidably adds cold hydrogen or cold oil expense and corresponding administration fee is used；Secondly, the unsaturated hydrocarbons such as the colloid contained in coal tar and aromatic hydrocarbon, hydrogenation process is susceptible to condensation, coking, especially when adopting fixed bed hydrogenation PROCESS FOR TREATMENT coal tar, particularly high temperature coal-tar, unsaturated hydrocarbons polycondensation green coke meeting blocking catalyst bed, cause catalyst surface carbon distribution, bed porosity declines, in turn result in rapid increase in the bed pressure drop short time, device is had to carry out shut-down and is changed agent, has a strong impact on device service cycle, and how solving this difficult problem becomes one of difficult problem that puzzlement enterprise produces；On the other hand, the fraction after coal tar hydrogenating process still suffers from substantial amounts of unsaturated hydrocarbons, causes product defective, cause that Petroleum virtue is dived high, diesel oil distillate Cetane number only has about 20, and these fractions do not reach product requirement, it is therefore desirable to carry out further hydrotreatment.
In boiling bed hydrogenation technology, in reactor, hydrogen, catalyst and oil sample are fluidized state, and whole bed temperature is homogeneous, pressure drop is little, and heat and mass is good, it is possible to advantageously promote the carrying out of hydrogenation reaction；Additionally due to there is no traditional bed, so inferior raw material when carrying out hydrogenation reaction substantially without causing the accidents such as bed blocking, pressure drop rise, cycle of operation can be greatly prolonged, widen the scope of processing raw material, especially the inferior raw material for coking easy in coal tar wet goods hydrogenation process, this technology more can highlight its advantage；
Patent ZL02122573.7 describes a kind of coal tar heavy fractioning boiling bed hydrogenation cracking method and system; it is that full fraction of coal tar is first removed after less than C5 lighter hydrocarbons through flash distillation; hydrofinishing is carried out again by 4 switch protecting reactors; subsequently into boiling bed hydrogenation reactor; under MoO3-WO3 NiO-P TiO2 catalyst action; hydrogenation reactor inlet pressure is not more than 15.0MPa(hydrogen dividing potential drop); initial reaction temperature is 300～390 DEG C (beds mean temperatures), volume space velocity 0.4～4.0h-1, hydrogen to oil volume ratio 500～3000Nm3/m3.This production method is fixing bed and ebullated bed process integration process, but due to impurity content height in tar, and under high temperature, react easy coking, cause that beds clogging is serious, will keep long-term operation, it is necessary to often more catalyst changeout, catalyst amount is big, adds cost, complex process；Additionally, the excision of light component is first removed by this technique, in a disguised form making feed stock qualitative change weight, actual processing is the heavy constituent in coal tar.
Summary of the invention
For the deficiencies in the prior art, the present invention provides a kind of full fraction of coal tar hydrotreating method, described processing method both can ensure that full fraction of coal tar obtained hydro-conversion in fluidized bed reactor, the heat of release in coal tar hydrogenating process can be made full use of again, can ensure that coal tar hydrogenating product processes further simultaneously and obtain qualified products.
Hydrotreatment method for coal tar of the present invention includes herein below:
(1) enter hydrogenation reactor ebullating bed reactor district after coal tar and hydrogen mixing, under boiling-bed catalyst exists, carry out hydrogenation reaction；
(2) product that step (1) obtains is after flash-evaporation dehydration, is fractionated into obtaining light component and heavy constituent；
(3) step (2) separates the heavy constituent obtained and all returns to ebullating bed reactor district, or part returns to ebullating bed reactor district and mixes with fresh coal tar, throws away device outside remainder heavy constituent；
(4) step (2) separates the light component obtained and enters the fixed bed reaction district of hydrogenation reactor, under fixed bed hydrogenation catalyst exists, carries out hydrogenation reaction, and product is fractionated into obtaining gas, Petroleum and diesel oil；
Wherein, described hydrogenation reactor is concentric circular barrel reactor, described reactor includes inner layer cylinder and outer layer cylinder, described inner layer cylinder is ebullating bed reactor district, outer layer cylinder is fixed bed reaction district, ebullating bed reactor district does not connect each other with fixed bed reaction district, the reaction compartment being independent from, and is respectively equipped with feeding line and discharging pipeline.
In the inventive method, in step (2), light component and heavy constituent cutting temperature are 320 DEG C～400 DEG C, it is preferred to 340 DEG C～360 DEG C, it is possible to suitably regulate the cutting temperature of weight component according to feedstock property and ebullating bed reactor district temperature rise situation.
In the inventive method, heavy constituent part described in step (3) returns to ebullating bed reactor district and mixes with fresh coal tar, throws away device, wherein outside remainder heavy constituent, the heavy constituent returning to ebullating bed reactor district is attached most importance to the 40%～80% of component weight, it is preferred to 50%～70%.
In the inventive method, described in step (3), the reaction condition in ebullating bed reactor district is: reaction temperature 300 DEG C～400 DEG C, it is preferred to 340 DEG C～380 DEG C, reaction pressure 8～18MPa, it is preferred to 10～16MPa, volume space velocity 0.2～8.0h-1, it is preferred to 0.4～4.0h-1, hydrogen to oil volume ratio 100:1～1500:1, it is preferred to 600:1～1200:1.
In the inventive method, described in step (4), the operating condition in fixed bed reaction district is: reaction temperature 240～380 DEG C, it is preferred to 280～340 DEG C, reaction pressure 3～18MPa, it is preferred to 8～16MPa, volume space velocity 0.1～4.0h-1, it is preferred to 0.4～2.0h-1, hydrogen to oil volume ratio 100:1～1500:1, it is preferred to 500:1～1300:1
In the inventive method, ebullating bed reactor district adds fresh catalyst from top, discharges decaying catalyst from bottom.
In the inventive method, fixed bed reaction district filling Hydrobon catalyst, generally with silicon-containing alumina or aluminium oxide for carrier, with group VIB and/or group VIII metal for active metal component, the preferred molybdenum of group VIB and/or tungsten, the VIIIth preferred cobalt of race is or/and nickel.In described Hydrobon catalyst, group VIII metal content is calculated as 2wt% ~ 12wt% with oxide, and group VIB tenor is calculated as 5wt% ~ 25wt% with oxide.Described Hydrobon catalyst can be prepared by prior art, it is also possible to selects business Hydrobon catalyst.FDS-4A, 481-3, FH-40 etc. that business Hydrobon catalyst such as Fushun Petrochemical Research Institute develops.
In the inventive method, described boiling-bed catalyst is the hydrofinishing microspheric catalyst of the water resistant developed for coal tar, with group VIB and group VIII metal for active metal component, the wherein preferred molybdenum of group VIB and/or tungsten, the preferred cobalt of group VIII metal is or/and nickel, metal active constituent is one or more in cobalt, nickel, molybdenum, tungsten, catalyst for refining can contain auxiliary agent, one or more in K, P, Mg, Zr and Ca, group VIII metal content is calculated as 3wt% ~ 10wt% with oxide, and group VIB tenor is calculated as 6wt% ~ 30wt% with oxide.
In the inventive method, the light component that coal tar hydrogenating aftercut obtains is before entering fixed bed reaction district and carrying out hydrogenation reaction, heating furnace need not be additionally set, rely on the heat of coal tar hydrogenating release in ebullating bed reactor district that namely light component temperature can be promoted to reaction temperature required, therefore, a heating furnace can be saved, reduce equipment investment.
Compared with prior art, in the inventive method, adopt hydrogenation reactor, adopt the mode in ebullating bed reactor district and fixed bed reactors combination, take full advantage of the unsaturated hydrocarbons contained in coal tar and can discharge amount of heat in hydrogenation process, these heats are used for the light component heating fixed bed reaction district to reaction temperature, not only can effectively alleviate the temperature rise in ebullating bed reactor district, reduce the consumption of quench oil, and may be omitted with the heating furnace that in prior art, light component fixed bed reaction district hydrogenation is required, save equipment investment.In the inventive method, ebullating bed reactor district hydrogenation effluent separates the heavy constituent obtained and returns to ebullating bed reactor district, reacts, it is possible to improve ebullating bed reactor district feed properties, it is possible to slow down the operating severity in ebullating bed reactor district together with after mixing with fresh coal tar.And the inventive method can farthest obtain light-weight fuel oil, improves value-added content of product.First coal tar raw material carries out hydrogenation reaction in fluidized bed reactor, remove most metal, sulfur and asphalitine etc., then enter back into fixed bed reactors and carry out hydrogenation reaction, it is possible to reduce the problems such as the bed pressure drop rising that causes because of coking, extension fixture service cycle.Full fraction of coal tar can realize hydro-conversion in fluidized bed reactor, changeable reactor need not be pre-set or distillation column carries out fractional distillation, improve resource utilization, reduce energy consumption, higher coal tar conversion ratio can be realized, realize substantially not producing or producing heavy constituent less, the target of light oil with high yield as far as possible.
Accompanying drawing explanation
Fig. 1 is Hydrotreatment method for coal tar process chart of the present invention.
Detailed description of the invention
nullAs shown in Figure 1，Coal tar raw material 1 is in heat exchanger 9 place and the effluent heat exchange of ebullating bed reactor district，The ebullating bed reactor district 5 of hydrogenation reactor 4 is entered with the heated stove 3 of new hydrogen 2 after heating after heat exchange，Hydrogenation reaction is carried out under boiling-bed catalyst effect，Boiling bed hydrogenation reaction effluent 7 enters in flash tank 8，With coal tar raw material heat exchange after the light components such as moisture are removed，Light component 11 and heavy constituent 12 is obtained subsequently into fractionating column 10 carries out just fractional distillation，Light component 11 and new hydrogen 2 are mixed into the fixed bed reaction district 6 of hydrogenation reactor 4，Hydrofining reaction is carried out under fixed bde catalyst effect，Reaction effluent enters fractionating column 14 and carries out fractional distillation，Obtain lighter hydrocarbons 17，Petroleum 15 and qualified diesel oil 16，Heavy constituent 12 enters fluidized bed reactor after mixing with fresh coal tar raw material 1 and reacts.
Further illustrate the present invention program below by specific embodiment, but be not limited to described embodiment.
The coal tar raw material character that test adopts is listed in table 1 respectively, and test technology flow process is with reference to shown in Fig. 1, and reaction condition is in Table 2.Adopting the microspheric catalyst of Fushun Petrochemical Research Institute's exploitation, the tungsten-Raney nickel being carrier with aluminium oxide in compound reactor ebullating bed reactor district, wherein in catalyst, nickeliferous 6wt%(presses NiO calculating), tungstenic 12wt%(presses WO3Calculate).Catalyst particle diameter is 0.5mm, and bulk density is 0.79g/cm3, specific surface area is 260m2/g；The FH-40B catalyst in the FH series of Fushun Petrochemical Research Institute academy exploitation, the molybdenum-Raney nickel being carrier with aluminium oxide, wherein nickel oxide 4.5wt% in catalyst, molybdenum oxide 8.5wt% is adopted in fixed bed reactors space.
Table 1 coal tar raw material character
Embodiment 1～3
This embodiment adopts flow process shown in Fig. 1, and test raw material is coal tar described in table 1, and reaction condition is in Table 2, and reaction result is referring to table 3.
Comparative example 1
Adopt conventional coal tar boiling bed hydrogenation fixed bed hydrogenation group technology, namely full fraction of coal tar first passes through fluidized bed reactor, then fractional distillation obtains light component and heavy constituent, light component passes through fixed bed hydrogenation reactor, heavy constituent returns fluidized bed reactor, reaction condition is referring to table 2, and result of the test is referring to table 3.
Table 2 reaction condition
Table 3 reaction result
By real-world operation result it can be seen that when adopting compound reactor hydrogenation combination technique to process coal tar, fluidized bed reactor can effectively slow down beds coking and blocking, extension fixture service cycle,；Secondly, utilize coal tar hydrogenating exothermic heat of reaction amount can promote the light component temperature of hydrogenation to reaction temperature, make reaction bed Temperature Distribution as far as possible uniformly, make catalyst play maximum effect；Hydrofining reaction can obtain qualified petrol and diesel oil component, decreases quenching hydrogen or quench oil injection rate, saves a heating furnace, saves energy consumption.All in all, this process is that reconstructed coal tar provides a path for transformation.
Claims (10)
1. a Hydrotreatment method for coal tar, described method includes following content:
(1) enter hydrogenation reactor ebullating bed reactor district after coal tar and hydrogen mixing, under boiling-bed catalyst exists, carry out hydrogenation reaction；
(2) product that step (1) obtains is after flash-evaporation dehydration, is fractionated into obtaining light component and heavy constituent；
(3) step (2) separates the heavy constituent obtained and all returns to ebullating bed reactor district, or part returns to ebullating bed reactor district and mixes with fresh coal tar, throws away device outside remainder heavy constituent；
(4) step (2) separates the light component obtained and enters the fixed bed reaction district of hydrogenation reactor, under fixed bed hydrogenation catalyst exists, carries out hydrogenation reaction, and product is fractionated into obtaining gas, Petroleum and diesel oil；
Wherein, described hydrogenation reactor is concentric circular barrel reactor, described reactor includes inner layer cylinder and outer layer cylinder, described inner layer cylinder is ebullating bed reactor district, outer layer cylinder is fixed bed reaction district, ebullating bed reactor district does not connect each other with fixed bed reaction district, the reaction compartment being independent from, and is respectively equipped with feeding line and discharging pipeline.
2. in accordance with the method for claim 1, it is characterised in that: described in step (2), light component and heavy constituent cutting temperature are 320 DEG C～400 DEG C.
3. in accordance with the method for claim 2, it is characterised in that: described in step (2), light component and heavy constituent cutting temperature are 340 DEG C～360 DEG C.
4. in accordance with the method for claim 1, it is characterised in that: heavy constituent part described in step (3) returns to ebullating bed reactor district and mixes with fresh coal tar, throws away device outside remainder heavy constituent.
5. in accordance with the method for claim 4, it is characterised in that: the heavy constituent returning to ebullating bed reactor district described in step (3) is attached most importance to the 40%～80% of component weight, it is preferred to 50%～70%.
6. in accordance with the method for claim 1, it is characterised in that: described in step (1), the reaction condition of boiling bed hydrogenation reaction zone is: reaction temperature 300 DEG C～400 DEG C, reaction pressure 8～18MPa, volume space velocity 0.2～8.0h-1, hydrogen to oil volume ratio 100:1～1500:1.
7. the method described in claim 1 or 5, it is characterised in that: described in step (1), the reaction condition of boiling bed hydrogenation reaction zone is: reaction temperature 340 DEG C～380 DEG C, reaction pressure 10～16MPa, volume space velocity 0.4～4.0h-1, hydrogen to oil volume ratio 600:1～1200:1.
8. in accordance with the method for claim 1, it is characterised in that: described in step (3), the operating condition of fixed bed hydrogenation reaction zone is: reaction temperature 240～380 DEG C, reaction pressure 3～18MPa, volume space velocity 0.1～4.0h-1, hydrogen to oil volume ratio 100:1～1500:1.
9. the method described in claim 1 or 7, it is characterised in that: described in step (3), the operating condition of fixed bed hydrogenation reaction zone is: reaction temperature 280～340 DEG C, reaction pressure 8～16MPa, volume space velocity 0.4～2.0h-1, hydrogen to oil volume ratio 500:1～1300:1.
10. in accordance with the method for claim 1, it is characterised in that: ebullating bed reactor district adds fresh catalyst from top, discharges decaying catalyst from bottom.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107674703A (en) * | 2017-11-07 | 2018-02-09 | 河北新启元能源技术开发股份有限公司 | Reaction feed temperature control equipment in a kind of coal tar hydrogenating |
| CN112705117A (en) * | 2019-10-25 | 2021-04-27 | 中国石油化工股份有限公司 | Liquid phase hydrogenation reactor and hydrogenation process |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107674703A (en) * | 2017-11-07 | 2018-02-09 | 河北新启元能源技术开发股份有限公司 | Reaction feed temperature control equipment in a kind of coal tar hydrogenating |
| CN107674703B (en) * | 2017-11-07 | 2019-10-22 | 河北新启元能源技术开发股份有限公司 | Reaction feed temperature control equipment in a kind of coal tar hydrogenating |
| CN112705117A (en) * | 2019-10-25 | 2021-04-27 | 中国石油化工股份有限公司 | Liquid phase hydrogenation reactor and hydrogenation process |
| CN112705117B (en) * | 2019-10-25 | 2022-07-12 | 中国石油化工股份有限公司 | Liquid phase hydrogenation reactor and hydrogenation process |
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