CN113755209A - Device and method for step-by-step hydrogenation of coal tar cutting fraction - Google Patents
Device and method for step-by-step hydrogenation of coal tar cutting fraction Download PDFInfo
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- CN113755209A CN113755209A CN202111127317.8A CN202111127317A CN113755209A CN 113755209 A CN113755209 A CN 113755209A CN 202111127317 A CN202111127317 A CN 202111127317A CN 113755209 A CN113755209 A CN 113755209A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G65/00—Treatment of hydrocarbon oils by two or more hydrotreatment processes only
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2400/00—Products obtained by processes covered by groups C10G9/00 - C10G69/14
- C10G2400/04—Diesel oil
Abstract
The invention provides a device and a method for step-by-step hydrogenation of coal tar cutting fractions, wherein the device comprises a solvent oil hydrogenation unit, a first separation unit, a hydrofining unit, a second separation unit and a hydrocracking unit; an outlet of the solvent oil hydrogenation unit is sequentially connected with the first separation unit and the hydrofining unit, and a hydrogen supply solvent is extracted from an outlet at the lower part of the first separation unit; the outlet of the hydrofining unit is connected with the second separation unit, the wax oil fraction outlet of the second separation unit is connected with the inlet of the hydrocracking unit, and the outlet of the second separation unit is connected back to the second separation unit. The device provided by the invention utilizes the characteristic of coal tar cutting fraction to carry out hydrogenation step by step, the hydrogen donor solvent is prepared from the solvent naphtha fraction, then the light components are sequentially subjected to hydrorefining and hydrocracking to prepare various distillate oils, the yield and quality of the oil products are higher, and the utilization value of the coal tar is fully improved; the device has the advantages of simple structure, cyclic utilization of raw materials, and low energy consumption and cost.
Description
Technical Field
The invention belongs to the technical field of coal chemical industry, and relates to a device and a method for step-by-step hydrogenation of cut fractions of coal tar.
Background
Coal is used as an important fossil fuel and is a basic raw material of the current energy utilization technology, products produced by the method are various, the coal liquefaction reaction is one of the comprehensive utilization technologies of the coal, in the reaction process, the action of a solvent is crucial, and the coal slurry can be prepared by mixing the coal slurry with coal powder, so that a gas-liquid-solid three-phase reaction medium can be in a relatively stable and uniform state, and the liquefaction reaction is convenient to carry out; importantly, a large amount of active hydrogen can be released, free radical fragments generated by heating and cracking of the coal powder can be stabilized, and the condensation polymerization reaction is inhibited; therefore, the hydrogen donor solvent has obvious effect in the coal liquefaction reaction, and the source and preparation of the hydrogen donor solvent are one of the research hotspots in the coal chemical industry.
Coal tar is an important oil product obtained by pyrolyzing pulverized coal, has complex components, can reduce the resource value of the coal tar when directly used as fuel, and is easy to pollute the environment, so that the coal tar is usually subjected to fraction cutting so as to be convenient for respective utilization of various fractions, one fraction can be used as solvent oil to prepare a hydrogen supply solvent through hydrogenation, and the utilization value of the coal tar is improved by combining hydrogenation processes of other fractions.
CN 106635159A discloses a high solid content coal tar suspension bed hydrogenation system and process, and the system includes: a hydrogen gas supply unit; a catalyst supply unit; the device comprises a coal tar cutting unit, a hydrogen supply solvent pre-liquid separation unit and a hydrogen supply solvent pre-liquid separation unit, wherein the coal tar cutting unit is used for cutting high-solid-content coal tar into a first light component, a hydrogen supply solvent pre-liquid and a first heavy component; the hydrogen supply solvent preparation unit is respectively connected with the coal tar cutting unit and the hydrogen supply unit; the catalytic hydrogenation reaction unit is respectively connected with the coal tar segmentation unit, the hydrogen supply solvent preparation unit and the catalyst supply unit; the system emphasizes that the heavy components of the coal tar are hydrogenated by adopting a suspension bed reactor, and the preparation of a hydrogen supply solvent and the further utilization of byproducts are not clear.
CN 110003949A discloses a production device and a preparation method of a hydrogen donor solvent, wherein the production device comprises a hydrogen donor unit, a raw oil supply unit, a hydrogenation reaction unit, a separation unit and a stripping tower; the hydrogen supply unit comprises a hydrogen heating furnace and is connected with an inlet of the hydrogenation reaction unit, the separation unit comprises a first separator and a second separator, a first bottom discharge hole is connected with an inlet of the second separator, and a top discharge hole and a second bottom discharge hole which are arranged on the second separator are independently connected with the stripping tower. The production device only relates to a process of preparing the hydrogen donor solvent by hydrogenating one of the coal tar fractions, does not relate to the utilization of the hydrogen donor solvent by-product, and does not relate to the comprehensive utilization of the hydrogen donor solvent by-product and other fractions of the coal tar.
In conclusion, aiming at the comprehensive utilization of the coal tar distillate, particularly the solvent oil, a proper hydrogenation device and a proper hydrogenation process are selected according to the composition of the coal tar distillate, and the utilization value of the coal tar is improved and the qualified oil products are produced through the step-by-step processing of the product and the distillate.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a device and a method for step-by-step hydrogenation of coal tar cut fractions.
In order to achieve the purpose, the invention adopts the following technical scheme:
in one aspect, the invention provides a device for stepwise hydrogenation of coal tar cutting fractions, which comprises a solvent oil hydrogenation unit, a first separation unit, a hydrofining unit, a second separation unit and a hydrocracking unit; a first distillate oil inlet is formed in the solvent oil hydrogenation unit, an outlet of the solvent oil hydrogenation unit is connected with an inlet of the first separation unit, an upper outlet of the first separation unit is connected with an inlet of the hydrofining unit, and a lower outlet of the first separation unit is used for extracting a hydrogen supply solvent;
the hydrofining unit is also provided with a second distillate oil inlet, an outlet of the hydrofining unit is connected with an inlet of the second separation unit, different outlets of the second separation unit respectively extract gas-phase products, naphtha fractions, diesel fractions and wax oil fractions, a wax oil fraction outlet of the second separation unit is connected with an inlet of the hydrocracking unit, and an outlet of the hydrocracking unit is connected back to the inlet of the second separation unit.
According to the invention, as the coal tar is complex in component and high in direct processing difficulty, all components are respectively utilized after the coal tar is subjected to fraction cutting, the solvent oil fraction can be used for rapidly preparing a hydrogen supply solvent due to the composition characteristics of the solvent oil fraction, and relevant bond effects are involved in processes such as coal liquefaction reaction and the like; the device has the advantages of simple structure, cyclic utilization of raw materials, and low energy consumption and cost.
The following technical solutions are preferred technical solutions of the present invention, but not limited to the technical solutions provided by the present invention, and technical objects and advantageous effects of the present invention can be better achieved and achieved by the following technical solutions.
As a preferable technical scheme of the invention, the inlet of the solvent oil hydrogenation unit is connected with a hydrogen supply unit.
Preferably, the hydrogen supply unit comprises a hydrogen heating furnace.
Preferably, the first distillate inlet is connected to a first feed pump.
Preferably, the solvent oil hydrogenation unit comprises a first solvent oil hydrogenation reactor and a second solvent oil hydrogenation reactor, and an outlet of the first solvent oil hydrogenation reactor is connected with an inlet of the second solvent oil hydrogenation reactor.
In the invention, the coal tar distillate is divided according to the different boiling points of the distillate, so that the coal tar distillate can be subjected to targeted treatment according to the characteristics of each component, and the utilization value of the raw materials is improved.
In the invention, the first distillate oil is solvent oil fraction which is a middle fraction cut from coal tar, and the content of naphthenic aromatic hydrocarbon, aromatic carbon rate, density of solvent oil, hydrogen-carbon atomic ratio and the like in the solvent oil can be improved through hydrogenation reaction, and the first distillate oil is used as a hydrogen supply solvent to reduce the hydrogenation difficulty.
As a preferable technical scheme of the invention, the first separation unit comprises a hot high-pressure separator and a stabilizing tower, an outlet of the solvent oil hydrogenation unit is connected with an inlet of the hot high-pressure separator, an upper outlet of the hot high-pressure separator is connected with an inlet of the hydrofining unit, a lower outlet of the hot high-pressure separator is connected with an inlet of the stabilizing tower, an upper outlet of the stabilizing tower is connected with an inlet of the hydrofining unit, and a lower outlet of the stabilizing tower is used for extracting a hydrogen supply solvent.
Preferably, the stabilizer column is a fractionation column.
Preferably, the overhead component of the stabilizer column and the second distillate are both connected to the inlet of the hydrofinishing unit via a second feed pump.
In the invention, the solvent oil is hydrogenated, the product of the solvent oil needs to be separated and purified, a gas phase is separated by a hot high-pressure separator, a liquid phase is fractionated in a stabilizing tower, a qualified hydrogen supply solvent is obtained at the bottom of the tower, and a light component is separated at the top of the tower.
Preferably, the hydrofining unit comprises a first hydrofining reactor and a second hydrofining reactor, and the outlet of the first hydrofining reactor is connected with the inlet of the second hydrofining reactor.
As a preferable technical scheme of the invention, the second separation unit comprises a degassing tower and a fractionating tower, wherein the lower outlet of the degassing tower is connected with the inlet of the fractionating tower, the upper outlet of the degassing tower is used for separating gas phase products, and the outlet of the fractionating tower sequentially produces naphtha fraction, diesel fraction and wax oil fraction from top to bottom.
Preferably, the gas phase product comprises hydrogen sulphide, hydrogen and dry gas, the dry gas being a hydrocarbon gas having a total content of methane and ethane above 90%.
Preferably, the wax oil fraction outlet pipeline on the fractionating tower is divided into two branches, one branch is used for producing the wax oil fraction, and the other branch is connected to the inlet of the hydrocracking unit.
In the invention, the light fraction obtained by cutting the coal tar and the light component left after hydrogenation of the solvent oil are both subjected to hydrofining treatment, which is an important step of coal tar lightening, so that light oil and heavy oil products are obtained, and gas phase components are obtained at the same time, and desulfurization treatment can be carried out due to sulfur.
As a preferred technical scheme of the invention, a gas phase inlet of the hydrocracking unit is connected with an upper outlet of the hot high-pressure separator.
Preferably, the lower outlet of the hydrocracking unit is connected to the inlet of the second separation unit forming a recycle.
On the other hand, the invention provides a method for performing step hydrogenation on coal tar cutting fraction by using the device, which comprises the following steps:
(1) carrying out solvent oil hydrogenation reaction on first distillate oil obtained after cutting coal tar, and separating to obtain a light component and a hydrogen donor solvent;
(2) mixing the light component obtained in the step (1) with second distillate oil cut from coal tar, performing hydrofining reaction, and separating to obtain a gas-phase product, a naphtha fraction, a diesel fraction and a wax oil fraction;
(3) and (3) carrying out hydrocracking reaction on the wax oil fraction obtained in the step (2), and separating a reaction product from a hydrofining reaction product in the step (2).
In a preferred embodiment of the present invention, the first distillate of step (1) has a cut boiling range of 220 to 460 ℃, for example, 220 ℃, 250 ℃, 270 ℃, 300 ℃, 320 ℃, 360 ℃, 400 ℃, 425 ℃ or 460 ℃, but is not limited to the values listed, and other values not listed in the range of the values are also applicable.
Preferably, the first distillate in step (1) is first mixed with hot hydrogen at a temperature of from 50 to 150 ℃, such as 50 ℃, 60 ℃, 80 ℃, 100 ℃, 120 ℃ or 150 ℃ and the like, and then raised to 150 to 300 ℃, such as 150 ℃, 180 ℃, 200 ℃, 225 ℃, 250 ℃, 270 ℃ or 300 ℃ and the like, but not limited to the recited values, and other non-recited values within the range of the recited values are also applicable.
Preferably, the temperature before the hot hydrogen gas is mixed is 200 to 380 ℃, for example, 200 ℃, 220 ℃, 250 ℃, 270 ℃, 300 ℃, 320 ℃, 350 ℃ or 380 ℃, but is not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the hydrogenation reaction of the solvent oil in the step (1) comprises a two-stage reaction.
Preferably, the temperature of the hydrogenation reaction of the solvent oil in the step (1) is 180 to 380 ℃, for example 180 ℃, 200 ℃, 220 ℃, 250 ℃, 270 ℃, 300 ℃, 320 ℃, 350 ℃ or 380 ℃, but not limited to the recited values, and other values in the range of the recited values are also applicable, preferably 200 to 380 ℃.
Preferably, the pressure of the hydrogenation reaction of the solvent oil in the step (1) is 12.0 to 20.0MPa, such as 12.0MPa, 14.0MPa, 15.0MPa, 16.0MPa, 18.0MPa or 20.0MPa, but not limited to the values listed, and other values not listed in the range of the values are also applicable, and preferably 12.0 to 18.0 MPa.
Preferably, the volume ratio of hydrogen to oil in the hydrogenation reaction of the solvent oil in the step (1) is 1000:1 to 3000:1, such as 1000:1, 1200:1, 1500:1, 1800:1, 2000:1, 2400:1, 2700:1 or 3000:1, but not limited to the recited values, and other values not recited in the range of the values are also applicable, preferably 1500:1 to 3000: 1.
Preferably, the liquid hourly volume space velocity of the solvent oil hydrogenation reaction in the step (1) is 0.2-1.2 h-1E.g. 0.2h-1、0.4h-1、0.6h-1、0.8h-1、1.0h-1Or 1.2h-1And the like, but not limited to the recited values, and other values not recited within the range of the recited values are also applicable, and preferably 0.2 to 1.0h-1。
As a preferred technical scheme of the invention, the separation in the step (1) comprises hot high-pressure separation and fractional distillation.
Preferably, the temperature of the hot high pressure separation is 220 to 320 ℃, such as 220 ℃, 240 ℃, 250 ℃, 270 ℃, 300 ℃ or 320 ℃, but not limited to the recited values, and other values not recited in the range of values are also applicable; the pressure is 11 to 18MPa, for example 11MPa, 12MPa, 14MPa, 15MPa, 16MPa or 18MPa, but the pressure is not limited to the values listed, and other values not listed in the numerical range are also applicable.
Preferably, the hot high-pressure separated gas-phase product is used for the hydrofinishing reaction of step (2), and the liquid-phase product is subjected to fractional distillation.
Preferably, the overhead temperature of the fractionation is from 100 to 150 ℃, for example 100 ℃, 110 ℃, 120 ℃, 130 ℃, 140 ℃ or 150 ℃, but is not limited to the recited values, and other values not recited within this range are equally applicable; the bottom temperature is 280 to 340 ℃, for example, 280 ℃, 290 ℃, 300 ℃, 310 ℃, 320 ℃, 330 ℃ or 340 ℃, but is not limited to the recited values, and other unrecited values within the range of the values are also applicable, wherein the bottom temperature is the extraction temperature of the hydrogen donor solvent.
Preferably, the pressure of the fractionation is-0.07 to 0.5MPa, such as-0.07 MPa, -0.05MPa, -0.02MPa, 0MPa, 0.1MPa, 0.2MPa, 0.3MPa, 0.4MPa, or 0.5MPa, but is not limited to the recited values, and other values not recited within the numerical range are equally applicable.
As a preferred embodiment of the present invention, the cut distillation range of the second distillate in step (2) is not more than 220 ℃, for example, 220 ℃, 210 ℃, 200 ℃, 190 ℃, 180 ℃, 160 ℃, or 150 ℃, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the volume ratio of the light fraction to the second distillate in step (2) is 1:4 to 1:2, such as 1:4, 1:3.5, 1:3, 1:2.5 or 1:2, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the hydrofinishing reaction of step (2) comprises a two-stage reaction.
Preferably, the temperature of the hydrorefining reaction in step (2) is 180 to 427 ℃, for example 180 ℃, 200 ℃, 250 ℃, 300 ℃, 350 ℃, 400 ℃ or 427 ℃, but is not limited to the recited values, and other values not recited in the range of the values are also applicable, preferably 180 to 400 ℃.
Preferably, the pressure of the hydrorefining reaction in step (2) is 10.0 to 17.0MPa, for example, 10.0MPa, 11.0MPa, 12.0MPa, 13.0MPa, 14.0MPa, 15.0MPa, 16.0MPa or 17.0MPa, but is not limited to the above-mentioned values, and other values not mentioned in the above-mentioned range are also applicable, and preferably 10.0 to 16.0 MPa.
Preferably, the hydrorefining reaction in step (2) has a hydrogen-oil volume ratio of 1000:1 to 3000:1, for example, 1000:1, 1200:1, 1500:1, 1800:1, 2000:1, 2400:1, 2700:1, 3000:1, and the like, but is not limited to the recited values, and other values not recited within the range of values are also applicable, preferably 1500:1 to 3000: 1.
Preferably, the liquid hourly volume space velocity of the hydrofining reaction in the step (2) is 0.15-1.0 h-1E.g. 0.15h-1、0.2h-1、0.4h-1、0.6h-1、0.8h-1Or 1.0h-1And the like, but not limited to the recited values, and other values not recited within the range of the recited values are also applicable, and preferably 0.2 to 0.8h-1。
Preferably, the separation in step (2) comprises gas-liquid separation and liquid-phase fractionation.
Preferably, the gas-liquid separation temperature is 220 to 320 ℃, for example 220 ℃, 240 ℃, 260 ℃, 280 ℃, 300 ℃ or 320 ℃, but is not limited to the recited values, and other values not recited in the numerical range are also applicable; the pressure is 11 to 18MPa, for example 11MPa, 12MPa, 14MPa, 15MPa, 16MPa or 18MPa, but the pressure is not limited to the values listed, and other values not listed in the numerical range are also applicable.
Preferably, the gas phase product obtained by gas-liquid separation comprises hydrogen sulfide, hydrogen and dry gas.
Preferably, the liquid phase fractionation is carried out in a fractionating column, with a naphtha fraction at the top, a diesel fraction at the middle side and a wax oil fraction at the bottom.
In a preferred embodiment of the present invention, the wax oil fraction subjected to the hydrocracking reaction in step (3) accounts for 60 to 90%, for example, 60%, 65%, 70%, 75%, 80%, 85%, or 90%, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
Preferably, the raw material hydrogen of the hydrocracking reaction in the step (3) comes from a gas-phase product separated by hot high pressure.
Preferably, the hydrocracking reaction in step (3) is carried out at a temperature of 350 to 410 ℃, for example 350 ℃, 360 ℃, 370 ℃, 380 ℃, 390 ℃, 400 ℃ or 410 ℃, but not limited to the recited values, and other values not recited in the range of the values are also applicable, preferably 360 to 405 ℃.
Preferably, the pressure of the hydrocracking reaction in the step (3) is 10.0 to 17.0MPa, for example, 10.0MPa, 11.0MPa, 12.0MPa, 13.0MPa, 14.0MPa, 15.0MPa, 16.0MPa or 17.0MPa, but is not limited to the recited values, and other values not recited in the numerical range are also applicable, and preferably 11.0 to 16.0 MPa.
Preferably, the hydrogen-to-oil ratio of the hydrocracking reaction in step (3) is 800:1 to 2000:1, such as 800:1, 1000:1, 1200:1, 1500:1, 1600:1, 1800:1, 2000:1, etc., but not limited to the recited values, and other values not recited in the above range are also applicable, preferably 1200:1 to 1800: 1.
Preferably, the liquid hourly volume space velocity of the hydrocracking reaction in the step (3) is 0.2-0.9 h-1E.g. 0.2h-1、0.3h-1、0.4h-1、0.5h-1、0.6h-1、0.7h-1、0.8h-1Or 0.9h-1And the like, but not limited to the recited values, and other values not recited within the range of the recited values are also applicable, and preferably 0.2 to 0.8h-1。
Compared with the prior art, the invention has the following beneficial effects:
(1) the device provided by the invention utilizes the characteristics of the cut fraction of the coal tar to carry out hydrogenation step by step, the solvent oil fraction is used for preparing a hydrogen donor solvent, and then the light component is sequentially subjected to hydrofining and hydrocracking to prepare various distillate oils, so that the yield and the quality of the oil product are higher, the utilization value of the coal tar is fully improved, and the yield of the light oil can reach more than 93% relative to the cut fraction of the coal tar;
(2) the device has simple structure, can recycle raw materials, ensures the continuous and stable operation of the device, and has lower energy consumption and cost.
Drawings
FIG. 1 is a schematic structural diagram of a device for stepwise hydrogenation of coal tar cutting fraction provided in example 1 of the present invention;
the method comprises the following steps of 1-hydrogen supply unit, 2-solvent oil hydrogenation unit, 21-first solvent oil hydrogenation reactor, 22-second solvent oil hydrogenation reactor, 3-hot high-pressure separator, 4-stabilizer, 5-hydrofining unit, 51-first hydrofining reactor, 52-second hydrofining reactor, 6-degassing tower, 7-fractionating tower and 8-hydrocracking unit.
Detailed Description
In order to better illustrate the present invention and facilitate the understanding of the technical solutions of the present invention, the present invention is further described in detail below. However, the following examples are only simple examples of the present invention and do not represent or limit the scope of the present invention, which is defined by the claims.
The following are typical but non-limiting examples of the invention:
example 1:
the embodiment provides a device for stepwise hydrogenation of coal tar cutting fraction, the structural schematic diagram of the device is shown in fig. 1, and the device comprises a solvent oil hydrogenation unit 2, a first separation unit, a hydrofining unit 5, a second separation unit and a hydrocracking unit 8; a first distillate oil inlet is formed in the solvent oil hydrogenation unit 2, an outlet of the solvent oil hydrogenation unit 2 is connected with an inlet of a first separation unit, an upper outlet of the first separation unit is connected with an inlet of a hydrofining unit 5, and a lower outlet of the first separation unit is used for extracting a hydrogen supply solvent;
the hydrofining unit 5 is further provided with a second distillate oil inlet, an outlet of the hydrofining unit 5 is connected with an inlet of a second separation unit, different outlets of the second separation unit respectively extract gas-phase products, naphtha fractions, diesel fractions and wax oil fractions, a wax oil fraction outlet of the second separation unit is connected with an inlet of a hydrocracking unit 8, and an outlet of the hydrocracking unit 8 is connected back to the inlet of the second separation unit.
The inlet of the solvent oil hydrogenation unit 2 is connected with a hydrogen supply unit 1, and the hydrogen supply unit 1 comprises a hydrogen heating furnace.
And the first distillate oil inlet is connected with a first feeding pump.
The solvent oil hydrogenation unit 2 comprises a first solvent oil hydrogenation reactor 21 and a second solvent oil hydrogenation reactor 22, wherein an outlet of the first solvent oil hydrogenation reactor 21 is connected with an inlet of the second solvent oil hydrogenation reactor 22.
The first separation unit comprises a hot high-pressure separator 3 and a stabilizing tower 4, an outlet of the solvent oil hydrogenation unit 2 is connected with an inlet of the hot high-pressure separator 3, an upper outlet of the hot high-pressure separator 3 is connected with an inlet of the hydrofining unit 5, a lower outlet of the hot high-pressure separator 3 is connected with an inlet of the stabilizing tower 4, an upper outlet of the stabilizing tower 4 is connected with an inlet of the hydrofining unit 5, and a lower outlet of the stabilizing tower 4 is used for extracting a hydrogen supply solvent.
The stabilizing tower 4 is a fractionating tower; and the tower top component of the stabilizing tower 4 and the second distillate are both connected with an inlet of the hydrofining unit 5 through a second feeding pump.
The hydrofining unit 5 comprises a first hydrofining reactor 51 and a second hydrofining reactor 52, and an outlet of the first hydrofining reactor 51 is connected with an inlet of the second hydrofining reactor 52.
The second separation unit comprises a degassing tower 6 and a fractionating tower 7, wherein the lower outlet of the degassing tower 6 is connected with the inlet of the fractionating tower 7, the upper outlet of the degassing tower 6 separates a gas-phase product, and the outlet of the fractionating tower 7 sequentially produces naphtha fraction, diesel fraction and wax oil fraction from top to bottom;
the gas phase products include hydrogen sulfide, hydrogen, and dry gas.
And a wax oil fraction outlet pipeline on the fractionating tower 7 is divided into two branches, one branch is used for extracting wax oil fraction, and the other branch is connected to an inlet of the hydrocracking unit 8.
The gas phase inlet of the hydrocracking unit 8 is connected with the upper outlet of the hot high-pressure separator 3.
The lower outlet of the hydrocracking unit 8 is connected to the inlet of the second separation unit to form a cycle.
Example 2:
the embodiment provides a device for stepwise hydrogenation of coal tar cutting fraction, which comprises a solvent oil hydrogenation unit 2, a first separation unit, a hydrofining unit 5, a second separation unit and a hydrocracking unit 8; a first distillate oil inlet is formed in the solvent oil hydrogenation unit 2, an outlet of the solvent oil hydrogenation unit 2 is connected with an inlet of a first separation unit, an upper outlet of the first separation unit is connected with an inlet of a hydrofining unit 5, and a lower outlet of the first separation unit is used for extracting a hydrogen supply solvent;
the hydrofining unit 5 is further provided with a second distillate oil inlet, an outlet of the hydrofining unit 5 is connected with an inlet of a second separation unit, different outlets of the second separation unit respectively extract gas-phase products, naphtha fractions, diesel fractions and wax oil fractions, a wax oil fraction outlet of the second separation unit is connected with an inlet of a hydrocracking unit 8, and an outlet of the hydrocracking unit 8 is connected back to the inlet of the second separation unit.
The inlet of the solvent oil hydrogenation unit 2 is connected with a hydrogen supply unit 1, and the hydrogen supply unit 1 comprises a hydrogen heating furnace.
And the first distillate oil inlet is connected with a first feeding pump.
The solvent oil hydrogenation unit 2 comprises a solvent oil hydrogenation reactor.
The first separation unit comprises a hot high-pressure separator 3 and a stabilizing tower 4, an outlet of the solvent oil hydrogenation unit 2 is connected with an inlet of the hot high-pressure separator 3, an upper outlet of the hot high-pressure separator 3 is connected with an inlet of the hydrofining unit 5, a lower outlet of the hot high-pressure separator 3 is connected with an inlet of the stabilizing tower 4, an upper outlet of the stabilizing tower 4 is connected with an inlet of the hydrofining unit 5, and a lower outlet of the stabilizing tower 4 is used for extracting a hydrogen supply solvent.
The stabilizing tower 4 is a fractionating tower; and the tower top component of the stabilizing tower 4 and the second distillate are both connected with an inlet of the hydrofining unit 5 through a second feeding pump.
The hydrofinishing unit 5 comprises a hydrofinishing reactor.
The second separation unit comprises a degassing tower 6 and a fractionating tower 7, wherein the lower outlet of the degassing tower 6 is connected with the inlet of the fractionating tower 7, the upper outlet of the degassing tower 6 separates a gas-phase product, and the outlet of the fractionating tower 7 sequentially produces naphtha fraction, diesel fraction and wax oil fraction from top to bottom;
the gas phase products include hydrogen sulfide, hydrogen, and dry gas.
And a wax oil fraction outlet pipeline on the fractionating tower 7 is divided into two branches, one branch is used for extracting wax oil fraction, and the other branch is connected to an inlet of the hydrocracking unit 8.
The gas phase inlet of the hydrocracking unit 8 is connected with the upper outlet of the hot high-pressure separator 3.
The lower outlet of the hydrocracking unit 8 is connected to the inlet of the second separation unit to form a cycle.
Example 3:
the embodiment provides a method for stepwise hydrogenation of coal tar cutting fraction, which is implemented by adopting the device in the embodiment 1, and comprises the following steps:
(1) mixing first distillate oil obtained after cutting coal tar with hot hydrogen at the temperature of 300 ℃, raising the temperature of the first distillate oil from 100 ℃ to 200 ℃, wherein the cutting distillation range of the first distillate oil is 300-400 ℃, and then carrying out two-stage solvent oil hydrogenation reaction, wherein the temperature of the solvent oil hydrogenation reaction is 280 ℃, the pressure is 16.0MPa, the volume ratio of hydrogen to oil is 2000:1, and the liquid hourly volume space velocity is 0.8h-1Performing thermal high-pressure separation and fractionation, wherein the temperature of the thermal high-pressure separation is 270 ℃, the pressure is 15MPa, the gas-phase product of the thermal high-pressure separation is used for the hydrofining reaction in the step (2), the liquid-phase product is subjected to fractionation, the temperature of the top of the fractionation is 120 ℃, the temperature of the bottom of the fractionation is 300 ℃, and the pressure of the fractionation is 0.2MPa, so as to obtain a light component and a hydrogen supply solvent;
(2) mixing the light component obtained in the step (1) with second distillate oil obtained after cutting coal tar, wherein the cutting distillation range of the second distillate oil is 150-200 ℃, and the light componentAnd the second distillate oil in a volume ratio of 1:3, and then carrying out two-stage hydrofining reaction, wherein the hydrofining reaction is carried out at the temperature of 300 ℃, the pressure of 13.0MPa, the hydrogen-oil volume ratio of 2000:1 and the liquid hourly space velocity of 0.5h-1Performing gas-liquid separation and liquid-phase fractionation, wherein the gas-liquid separation temperature is 270 ℃, the pressure is 15MPa, the obtained gas-phase product comprises hydrogen sulfide, hydrogen and dry gas, the liquid-phase fractionation is performed in a fractionating tower, naphtha fraction is obtained at the top of the fractionating tower, diesel fraction is obtained at the middle lateral line, and wax oil fraction is obtained at the bottom of the fractionating tower;
(3) carrying out hydrocracking reaction on 75% of the wax oil fraction obtained in the step (2), wherein the raw material hydrogen is a gas-phase product separated by heat and high pressure, the hydrocracking reaction temperature is 370 ℃, the pressure is 13.0MPa, the volume ratio of hydrogen to oil is 1500:1, and the liquid hourly volume space velocity is 0.5h-1And (3) separating the reaction product and the hydrofining reaction product in the step (2) together.
In the embodiment, the method is adopted to carry out step hydrogenation on the coal tar cutting fraction, so that the coal tar fraction can be fully utilized, the yield of the light oil can reach 94.2% relative to the coal tar cutting fraction, the oil quality is high, and the device can continuously and stably operate.
Example 4:
the embodiment provides a method for stepwise hydrogenation of coal tar cutting fraction, which is implemented by adopting the device in the embodiment 1, and comprises the following steps:
(1) mixing first distillate oil obtained after cutting coal tar with hot hydrogen at the temperature of 380 ℃, raising the temperature of the first distillate oil from 150 ℃ to 300 ℃, wherein the cutting distillation range of the first distillate oil is 350-460 ℃, and then carrying out two-stage solvent oil hydrogenation reaction, wherein the temperature of the solvent oil hydrogenation reaction is 360 ℃, the pressure is 20.0MPa, the volume ratio of hydrogen to oil is 1200:1, and the liquid hourly volume space velocity is 1.2h-1And (3) carrying out thermal high-pressure separation and fractionation, wherein the temperature of the thermal high-pressure separation is 320 ℃, the pressure is 18MPa, the gas-phase product of the thermal high-pressure separation is used for the hydrofining reaction in the step (2), the liquid-phase product is fractionated, the temperature of the top of the fractionation is 150 ℃, the temperature of the bottom of the fractionation is 340 ℃, and the pressure of the fractionation is 0.5MPa, obtaining light components and a hydrogen donor solvent;
(2) mixing the light component obtained in the step (1) with second distillate oil obtained after cutting of coal tar, wherein the cutting distillation range of the second distillate oil is 180-220 ℃, the volume ratio of the light component to the second distillate oil is 1:4, then carrying out two-stage hydrofining reaction, wherein the hydrofining reaction is at the temperature of 400 ℃, the pressure of 16.0MPa, the volume ratio of hydrogen to oil is 1200:1, and the liquid hourly volume space velocity is 1.0h-1Performing gas-liquid separation and liquid-phase fractionation, wherein the gas-liquid separation temperature is 320 ℃, the pressure is 18MPa, the obtained gas-phase product comprises hydrogen sulfide, hydrogen and dry gas, the liquid-phase fractionation is performed in a fractionating tower, naphtha fraction is obtained at the top of the fractionating tower, diesel fraction is obtained at the middle lateral line, and wax oil fraction is obtained at the bottom of the fractionating tower;
(3) performing hydrocracking reaction on 60% of the wax oil fraction obtained in the step (2), wherein the raw material hydrogen is a gas-phase product obtained by thermal high-pressure separation, the hydrocracking reaction temperature is 410 ℃, the pressure is 16.0MPa, the volume ratio of hydrogen to oil is 1000:1, and the liquid hourly volume space velocity is 0.9h-1And (3) separating the reaction product and the hydrofining reaction product in the step (2) together.
In the embodiment, the method is adopted to carry out step hydrogenation on the coal tar cutting fraction, so that the coal tar fraction can be fully utilized, the yield of the light oil can reach 93.8% relative to the coal tar cutting fraction, the oil quality is high, and the device can continuously and stably operate.
Example 5:
the embodiment provides a method for stepwise hydrogenation of coal tar cutting fraction, which is implemented by adopting the device in the embodiment 1, and comprises the following steps:
(1) mixing first distillate oil obtained after cutting coal tar with hot hydrogen at the temperature of 200 ℃, raising the temperature of the first distillate oil from 50 ℃ to 150 ℃, wherein the cutting distillation range of the first distillate oil is 220-320 ℃, and then carrying out two-stage solvent oil hydrogenation reaction, wherein the temperature of the solvent oil hydrogenation reaction is 200 ℃, the pressure is 12.0MPa, the volume ratio of hydrogen to oil is 3000:1, and the liquid hourly volume space velocity is 0.4h-1Subjected to thermal high-pressure separation and fractional distillation, said thermal high-pressure separationThe temperature of the step (2) is 220 ℃, the pressure of the step (2) is 12MPa, the gas-phase product of the thermal high-pressure separation is used for the hydrofining reaction of the step (2), the liquid-phase product is fractionated, the temperature of the top of the fractionation is 100 ℃, the temperature of the bottom of the fractionation is 280 ℃, and the pressure of the fractionation is-0.05 MPa, so that a light component and a hydrogen donor solvent are obtained;
(2) mixing the light component obtained in the step (1) with second distillate oil obtained after cutting of coal tar, wherein the cutting distillation range of the second distillate oil is 140-180 ℃, the volume ratio of the light component to the second distillate oil is 1:2, then carrying out two-stage hydrofining reaction, wherein the hydrofining reaction is carried out at the temperature of 200 ℃, the pressure of 10.0MPa, the volume ratio of hydrogen to oil is 3000:1, and the liquid hourly volume space velocity is 0.3h-1Performing gas-liquid separation and liquid-phase fractionation, wherein the gas-liquid separation temperature is 220 ℃, the pressure is 12MPa, the obtained gas-phase product comprises hydrogen sulfide, hydrogen and dry gas, the liquid-phase fractionation is performed in a fractionating tower, naphtha fraction is obtained at the top of the fractionating tower, diesel fraction is obtained at the middle lateral line, and wax oil fraction is obtained at the bottom of the fractionating tower;
(3) performing hydrocracking reaction on 90% of the wax oil fraction obtained in the step (2), wherein the raw material hydrogen is a gas-phase product obtained by thermal high-pressure separation, the hydrocracking reaction temperature is 350 ℃, the pressure is 10.0MPa, the volume ratio of hydrogen to oil is 2000:1, and the liquid hourly volume space velocity is 0.2h-1And (3) separating the reaction product and the hydrofining reaction product in the step (2) together.
In the embodiment, the method is adopted to carry out step hydrogenation on the coal tar cutting fraction, so that the coal tar fraction can be fully utilized, the yield of the light oil can reach 93.25 percent relative to the coal tar cutting fraction, the oil quality is high, and the device can continuously and stably operate.
Example 6:
the embodiment provides a method for stepwise hydrogenation of coal tar cutting fraction, which is implemented by adopting the device in the embodiment 2, and comprises the following steps:
(1) mixing first distillate oil obtained after cutting coal tar with hot hydrogen at the temperature of 250 ℃, wherein the temperature of the first distillate oil is increased from 80 ℃ to 200 ℃, the cutting distillation range of the first distillate oil is 250-350 ℃, and thenThen carrying out a solvent oil hydrogenation reaction, wherein the temperature of the solvent oil hydrogenation reaction is 250 ℃, the pressure is 18.0MPa, the volume ratio of hydrogen to oil is 1500:1, and the liquid hourly space velocity is 0.2h-1Performing thermal high-pressure separation and fractionation, wherein the temperature of the thermal high-pressure separation is 250 ℃, the pressure is 16MPa, the gas-phase product of the thermal high-pressure separation is used for the hydrofining reaction in the step (2), the liquid-phase product is subjected to fractionation, the temperature of the top of the fractionation is 135 ℃, the temperature of the bottom of the fractionation is 320 ℃, and the pressure of the fractionation is 0.1MPa, so as to obtain a light component and a hydrogen supply solvent;
(2) mixing the light component obtained in the step (1) with second distillate oil obtained after cutting of coal tar, wherein the cutting distillation range of the second distillate oil is 170-210 ℃, the volume ratio of the light component to the second distillate oil is 1:3, and then carrying out hydrofining reaction, wherein the temperature of the hydrofining reaction is 350 ℃, the pressure is 15.0MPa, the volume ratio of hydrogen to oil is 1500:1, and the liquid hourly volume space velocity is 0.15h-1Performing gas-liquid separation and liquid-phase fractionation, wherein the gas-liquid separation temperature is 300 ℃, the pressure is 14MPa, the obtained gas-phase product comprises hydrogen sulfide, hydrogen and dry gas, the liquid-phase fractionation is performed in a fractionating tower, naphtha fraction is obtained at the top of the fractionating tower, diesel fraction is obtained at the middle lateral line, and wax oil fraction is obtained at the bottom of the fractionating tower;
(3) carrying out hydrocracking reaction on 80% of the wax oil fraction obtained in the step (2), wherein the raw material hydrogen is a gas-phase product obtained by thermal high-pressure separation, the hydrocracking reaction temperature is 390 ℃, the pressure is 14.0MPa, the volume ratio of hydrogen to oil is 1600:1, and the liquid hourly volume space velocity is 0.4h-1And (3) separating the reaction product and the hydrofining reaction product in the step (2) together.
In the embodiment, the method is adopted to carry out step hydrogenation on the coal tar cutting fraction, so that the coal tar fraction can be fully utilized, the yield of the light oil can reach 93.0 percent relative to the coal tar cutting fraction, the oil quality is high, and the device can continuously and stably operate.
Comparative example 1:
this comparative example provides an apparatus and process for the step-wise hydrogenation of coal tar cut fractions, with reference to the apparatus of example 1, except that: hydrocracking unit 8 is not included.
The process is referred to the process in example 3, with the only difference that: step (3) is not included.
In the comparative example, the heavy components of the wax oil after hydrorefining the light components in the cut fraction of the coal tar are not subjected to hydrocracking, so that the yield of the light oil is reduced to only 70-75%, and the utilization value of the coal tar is not fully exerted.
It can be seen from the above examples and comparative examples that the device of the present invention utilizes the characteristics of the cut fraction of coal tar to perform hydrogenation step by step, prepares a hydrogen donor solvent from the solvent oil fraction, and then sequentially hydrofinishes and hydrocracks the light components to prepare various distillate oils, the yield and quality of oil products are high, the utilization value of coal tar is fully improved, and the yield of light oil can reach more than 93% relative to the cut fraction of coal tar; the device has the advantages of simple structure, cyclic utilization of raw materials, continuous and stable operation of the device, and low energy consumption and cost.
The applicant states that the present invention is illustrated by the detailed apparatus and method of the present invention through the above embodiments, but the present invention is not limited to the above detailed apparatus and method, i.e. it is not meant to imply that the present invention must be implemented by the above detailed apparatus and method. It will be apparent to those skilled in the art that any modifications to the present invention, equivalents of the means for substitution and addition of means for carrying out the invention, selection of specific means, etc., are within the scope and disclosure of the invention.
Claims (10)
1. The device for stepwise hydrogenation of cut fractions of coal tar is characterized by comprising a solvent oil hydrogenation unit, a first separation unit, a hydrofining unit, a second separation unit and a hydrocracking unit; a first distillate oil inlet is formed in the solvent oil hydrogenation unit, an outlet of the solvent oil hydrogenation unit is connected with an inlet of the first separation unit, an upper outlet of the first separation unit is connected with an inlet of the hydrofining unit, and a lower outlet of the first separation unit is used for extracting a hydrogen supply solvent;
the hydrofining unit is also provided with a second distillate oil inlet, an outlet of the hydrofining unit is connected with an inlet of the second separation unit, different outlets of the second separation unit respectively extract gas-phase products, naphtha fractions, diesel fractions and wax oil fractions, a wax oil fraction outlet of the second separation unit is connected with an inlet of the hydrocracking unit, and an outlet of the hydrocracking unit is connected back to the inlet of the second separation unit.
2. The device of claim 1, wherein the inlet of the solvent oil hydrogenation unit is connected with a hydrogen supply unit;
preferably, the hydrogen supply unit comprises a hydrogen heating furnace;
preferably, the first distillate oil inlet is connected with a first feeding pump;
preferably, the solvent oil hydrogenation unit comprises a first solvent oil hydrogenation reactor and a second solvent oil hydrogenation reactor, and an outlet of the first solvent oil hydrogenation reactor is connected with an inlet of the second solvent oil hydrogenation reactor.
3. The apparatus according to claim 1 or 2, wherein the first separation unit comprises a hot high-pressure separator and a stabilizer column, the outlet of the solvent oil hydrogenation unit is connected with the inlet of the hot high-pressure separator, the upper outlet of the hot high-pressure separator is connected with the inlet of the hydrofining unit, the lower outlet of the hot high-pressure separator is connected with the inlet of the stabilizer column, the upper outlet of the stabilizer column is connected with the inlet of the hydrofining unit, and the lower outlet of the stabilizer column produces a hydrogen supply solvent;
preferably, the stabilizer column is a fractionation column;
preferably, the overhead component and the second distillate of the stabilizer are both connected with the inlet of the hydrofining unit through a second feeding pump;
preferably, the hydrofining unit comprises a first hydrofining reactor and a second hydrofining reactor, and the outlet of the first hydrofining reactor is connected with the inlet of the second hydrofining reactor.
4. The apparatus according to any one of claims 1 to 3, wherein the second separation unit comprises a degassing tower and a fractionating tower, wherein a lower outlet of the degassing tower is connected with an inlet of the fractionating tower, an upper outlet of the degassing tower separates gas-phase products, and an outlet of the fractionating tower sequentially produces naphtha fraction, diesel fraction and wax oil fraction from top to bottom;
preferably, the gas phase product comprises hydrogen sulfide, hydrogen and dry gas;
preferably, the wax oil fraction outlet pipeline on the fractionating tower is divided into two branches, one branch is used for producing the wax oil fraction, and the other branch is connected to the inlet of the hydrocracking unit.
5. The apparatus according to any one of claims 1 to 4, characterized in that the gas phase inlet of the hydrocracking unit is connected to the upper outlet of the hot high pressure separator;
preferably, the lower outlet of the hydrocracking unit is connected to the inlet of the second separation unit forming a recycle.
6. A method for carrying out the step hydrogenation of the coal tar cutting fraction by using the device of any one of claims 1 to 5, which is characterized by comprising the following steps:
(1) carrying out solvent oil hydrogenation reaction on first distillate oil obtained after cutting coal tar, and separating to obtain a light component and a hydrogen donor solvent;
(2) mixing the light component obtained in the step (1) with second distillate oil cut from coal tar, performing hydrofining reaction, and separating to obtain a gas-phase product, a naphtha fraction, a diesel fraction and a wax oil fraction;
(3) and (3) carrying out hydrocracking reaction on the wax oil fraction obtained in the step (2), and separating a reaction product from a hydrofining reaction product in the step (2).
7. The method of claim 6, wherein the first distillate of step (1) has a cut distillation range of 220 to 460 ℃;
preferably, the first distillate oil in the step (1) is firstly mixed with hot hydrogen, and the temperature is increased from 50-150 ℃ to 150-300 ℃;
preferably, the temperature of the hot hydrogen before mixing is 200-380 ℃;
preferably, the hydrogenation reaction of the solvent oil in the step (1) comprises a two-stage reaction;
preferably, the temperature of the hydrogenation reaction of the solvent oil in the step (1) is 180-380 ℃;
preferably, the pressure of the hydrogenation reaction of the solvent oil in the step (1) is 12.0-20.0 MPa;
preferably, the volume ratio of hydrogen to oil in the hydrogenation reaction of the solvent oil in the step (1) is 1000: 1-3000: 1;
preferably, the liquid hourly volume space velocity of the solvent oil hydrogenation reaction in the step (1) is 0.2-1.2 h-1。
8. The process of claim 6 or 7, wherein the separating of step (1) comprises hot high pressure separation and fractional distillation;
preferably, the temperature of the hot high-pressure separation is 220-320 ℃, and the pressure is 11-18 MPa;
preferably, the hot high-pressure separated gas-phase product is used for the hydrofining reaction of the step (2), and the liquid-phase product is fractionated;
preferably, the temperature of the top of the fractionating tower is 100-150 ℃, and the temperature of the bottom of the fractionating tower is 280-340 ℃;
preferably, the pressure of the fractionation is-0.07 to 0.5 MPa.
9. The process of any of claims 6-8, wherein the second distillate of step (2) has a cut boiling range of no greater than 220 ℃;
preferably, the volume ratio of the light component to the second distillate oil in the step (2) is 1: 4-1: 2;
preferably, the hydrofining reaction of step (2) comprises a two-stage reaction;
preferably, the temperature of the hydrofining reaction in the step (2) is 180-427 ℃;
preferably, the pressure of the hydrofining reaction in the step (2) is 10.0-17.0 MPa;
preferably, the hydrogen-oil volume ratio of the hydrorefining reaction in the step (2) is 1000: 1-3000: 1;
preferably, the liquid hourly volume space velocity of the hydrofining reaction in the step (2) is 0.15-1.0 h-1Preferably 0.2 to 0.8h-1；
Preferably, the separation in step (2) comprises gas-liquid separation and liquid-phase fractionation;
preferably, the gas-liquid separation temperature is 220-320 ℃, and the pressure is 11-18 MPa;
preferably, the gas-phase product obtained by gas-liquid separation comprises hydrogen sulfide, hydrogen and dry gas;
preferably, the liquid phase fractionation is carried out in a fractionating column, with a naphtha fraction at the top, a diesel fraction at the middle side and a wax oil fraction at the bottom.
10. The method according to any one of claims 6 to 9, wherein the wax oil fraction subjected to the hydrocracking reaction in the step (3) accounts for 60 to 90%;
preferably, the raw material hydrogen of the hydrocracking reaction in the step (3) comes from a gas-phase product separated by hot high pressure;
preferably, the temperature of the hydrocracking reaction in the step (3) is 350-410 ℃;
preferably, the pressure of the hydrocracking reaction in the step (3) is 10.0-17.0 MPa;
preferably, the volume ratio of hydrogen to oil in the hydrocracking reaction in the step (3) is 800: 1-2000: 1, preferably 1200: 1-1800: 1;
preferably, the liquid hourly volume space velocity of the hydrocracking reaction in the step (3) is 0.2-0.9 h-1。
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