CN110003949A - A kind of process units and preparation method of hydrogen supply dissolvent - Google Patents
A kind of process units and preparation method of hydrogen supply dissolvent Download PDFInfo
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- CN110003949A CN110003949A CN201910380736.9A CN201910380736A CN110003949A CN 110003949 A CN110003949 A CN 110003949A CN 201910380736 A CN201910380736 A CN 201910380736A CN 110003949 A CN110003949 A CN 110003949A
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- hydrogen
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- stripper
- base oil
- oil
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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
- C10G67/00—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only
- C10G67/02—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only plural serial stages only
- C10G67/14—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only plural serial stages only including at least two different refining steps in the absence of hydrogen
Abstract
This application involves a kind of process units of hydrogen supply dissolvent and preparation method, the process units includes hydrogen supply unit, feedstock oil feed unit, hydrogenation reaction unit, separative unit and stripper；The preparation method mixes after including the following steps: feedstock oil heating with hydrogen, gas-liquid separation after hydrogenation reaction, obtains adding hydrogen base oil；Fractionation plus hydrogen base oil, base oil light component are fed by the stripper middle and upper part, and base oil heavy constituent is by charging in the middle part of the stripper；Base oil light component and base oil heavy constituent are stripped, obtains hydrogen supply dissolvent oil in stripper tower bottom.Gained hydrogen supply dissolvent is up to 20.82 for hydrogen index (HI), and hydrogen supply capacity is strong；The process flow of the hydrogen supply dissolvent preparation method is simple, by operating parameters such as control hydrogen-oil ratio, reaction temperature, reaction pressure, air speeds, prevents the supersaturation of hydrogen supply dissolvent, and the yield of hydrogen supply dissolvent is up to 88.64%.
Description
Technical field
The invention belongs to coal chemical technologies, are related to a kind of hydrogen supply dissolvent more particularly to a kind of process units of hydrogen supply dissolvent
And preparation method.
Background technique
Hydrogen supply dissolvent technique is the liquefaction process that coal is directly reacted with the hydrogen supply dissolvent of pre-add hydrogen, the work of hydrogen supply dissolvent
Coal is dispersed in coal slurry with being, and fluidization of coal conveying by reaction system, and provides that reactive hydrogen carries out coal plus hydrogen is anti-
It answers, hydrogen supply dissolvent can dissolve coal, and the free radical fragment polycondensation for preventing pyrolysis of coal from generating, to improve the receipts of liquefied coal coil
Rate；Hydrogen supply dissolvent can dissolve gas phase hydrogen, spread hydrogen molecule to coal or catalyst surface；Hydrogen supply dissolvent can also be to free radical
The direct hydrogen supply of fragment or transmitting hydrogen.
The high hydrogen supply dissolvent of hydrogen supply capacity, can promote the conversion of coal, to increase the yield of coal direct liquefaction oil, also
Conducive to the preparation, conveying and mobility of coal slurry.It is existing studies have shown that partially hydrogenated polycyclic aromatic hydrocarbon (such as naphthane, dihydro
Phenanthrene, dihydroanthracene, tetrahydro anthracene) there is very strong hydrogen supply capacity, saturated hydrocarbons does not have or with very weak hydrogen supply capacity.Produce one kind
The strong hydrogen supply dissolvent of hydrogen supply capacity is conducive to the conversion ratio for improving mink cell focus or coal tar pitch, improves light oil yield.
101370914 A of CN discloses a kind of method of hydrotreating of brown coal directly liquefied circulating solvent, is mainly characterized by
Under the process conditions of mitigation realize coal liquefaction solvent incomplete saturated hydrogenation, improve solvent for hydrogen amount.CN 1587351 A
Direct coal liquefaction process in, liquefied coal coil removes most of sulphur, nitrogen and nitrogen heteroatom after stabilized hydrogenation, prior
Partial hydrogenation saturation is carried out to aromatic hydrocarbons, improves the hydrogen supply capacity of circulation solvent.But due to the liquefied coal coil of DCL/Direct coal liquefaction production
In contain fractional saturation hydrocarbon, saturated hydrocarbon content further increases after hydrotreating, account for about circulation hydrogen supply dissolvent 30% or so,
This fractional saturation hydrocarbon does not have during DCL/Direct coal liquefaction or with very weak hydrogen supply capacity, to affect the conversion ratio of coal
And oil yield.
Using the saturated hydrocarbons containing high level in circulation hydrogen supply dissolvent made from prior art, this leads to circulation obtained
The hydrogen supply capacity of hydrogen supply dissolvent is poor, therefore it provides a kind of hydrogen supply dissolvent that hydrogen supply capacity is strong and its process units and method, right
Have great importance in coal liquefaction craft.
Summary of the invention
The purpose of the present invention is to provide a kind of process units of hydrogen supply dissolvent and preparation method, hydrogen supply provided by the invention
The hydrogen supply index of solvent reaches 20.82, and hydrogen supply capacity is strong；Process units structure provided by the invention is simple, and equipment investment is low；This
The process flow for inventing the hydrogen supply dissolvent preparation method provided is simple, passes through the setting of high pressure hot separator, thermal low-pressure separators
The supersaturation of hydrogen supply dissolvent is prevented, and the yield of hydrogen supply dissolvent is up to 88.64%.
In order to achieve that object of the invention, the invention adopts the following technical scheme:
In a first aspect, described device includes hydrogen supply unit, raw material the present invention provides a kind of process units of hydrogen supply dissolvent
Oily feed unit, hydrogenation reaction unit, separative unit and stripper.
The feedstock oil feed unit includes sequentially connected raw material oil tank, feedstock oil delivery pump, heat exchanger.
The hydrogen supply unit includes hydrogen heating furnace, the outlet and the entrance phase of hydrogenation reaction unit of the hydrogen heating furnace
Even, the connecting line between hydrogen heating furnace and hydrogenation reaction unit entrance is also connected with the outlet of the heat exchanger.
The separative unit includes the first separator and the second separator, and first separator is provided with top gas outlet
With the first bottom discharge port, the first bottom discharge port is connect with the entrance of second separator；The second separator setting
Have a top discharge mouth and the second bottom discharge port, the top discharge mouth and the second bottom discharge port separately with the vapour
Stripper connection.
The hydrogenation reaction unit includes at least one hydrogenator, is connected in series between the hydrogenator, most
The outlet of the latter hydrogenator is connect after the heat exchanger with the entrance of first separator.
Feedstock oil in the present invention in feedstock oil feed unit flows through heat exchanger under the action of feedstock oil delivery pump, heating
It is mixed afterwards with the hydrogen of hydrogen heating furnace outflow, and enters in hydrogenator reacted together, high temperature after reaction
Mixture flow is used to heat feedstock oil through heat exchanger, the gas-liquid separation in the first separator of the hot mixture after cooling, gas
It is discharged by top gas outlet, adds hydrogen base oil to flow into the second separator by the bottom discharge port of the first separator, and in the second separation
Fractionation is base oil light component and base oil heavy constituent in device, wherein base oil light component is fed by stripper middle and upper part, base oil heavy constituent
By feeding in the middle part of stripper, stripper bottom is passed through superheated steam for stripping base oil light component and base oil heavy constituent, and in vapour
Stripper bottom obtains hydrogen supply dissolvent.
Preferably, the hydrogenation reaction unit includes 2-5 hydrogenator, such as can be 2,3,4 or 5
It is a, preferably 2 hydrogenators.Increasing hydrogenator can be improved the conversion ratio of feedstock oil, but can make hydrogenation reaction at
Originally it is multiplied.Under the premise of considering hydrogenation reaction cost, temperature, pressure, hydrogen that the present invention passes through control hydrogenation reaction
Liquid hourly space velocity (LHSV) with the volume ratio of feedstock oil and when reacting, keeps the conversion ratio of feedstock oil higher, final gained plus hydrogen solvent
For hydrogen index (HI) height.
Preferably, the hydrogenator is fixed bed reactors.
Preferably, first separator is high pressure hot separator.Mixing in the present invention by being flowed out in hydrogenator
Object gas-liquid separation in high pressure hot separator, extra hydrogen are discharged by the top gas outlet of high pressure hot separator, are prevented excessive
Hydrogen makes plus the supersaturation of hydrogen solvent, while also increasing the yield for adding hydrogen solvent.
Preferably, second separator is thermal low-pressure separators.Flow out in first separator plus hydrogen base oil enters heat
It is fractionated in low pressure separator, gained base oil light component enters stripper top, and gained base oil heavy constituent enters in stripper
Portion.
Preferably, the stripper top is additionally provided with stripper return tank.
Stripper top gas phase flows into stripper return tank and the gas-liquid separation in stripper return tank in the present invention, does not coagulate
Gas is flowed out by outflow at the top of stripper return tank, water phase by stripper reflux pot bottom, and light oil phase a part is back to stripping
Top of tower adds the yield of hydrogen solvent to improve, and another part is mutually exported discharge by light oil.
Preferably, described device is additionally provided with hydrogen recovery unit, and the hydrogen recovery unit includes sequentially connected sky
Cooler, gas-liquid separator and compressor, the entrance of the air cooler are connect with the top gas outlet of first separator, institute
The gas vent for stating compressor is connect with the entrance of hydrogen heating furnace.
High temperature gas phase is flowed out by the top gas outlet of the first separator, enters gas-liquid separator, water after air cooler is cooling
It is mutually mutually flowed out by gas-liquid separator bottom with light oil, gained hydrogen enters hydrogen after compressor pressurizes and heats stove heating, so
It is mixed afterwards with feedstock oil.
Preferably, the water phase outlet of the gas-liquid separator and the water phase of the stripper return tank are exported and are connected.
Preferably, the light oil of the gas-liquid separator mutually exports and the light oil of the stripper return tank mutually company of outlet
It connects.
Second aspect, the present invention provides a kind of method that application device as described in relation to the first aspect prepares hydrogen supply dissolvent,
Described method includes following steps:
(1) feedstock oil and hydrogen after Hybrid Heating, gas-liquid separation after hydrogenation reaction obtain plus hydrogen base oil；
(2) fractionation plus hydrogen base oil, base oil light component are fed by the stripper top, and base oil heavy constituent is by the stripper
Middle part charging；
(3) stripping base oil light component and base oil heavy constituent obtain hydrogen supply dissolvent oil in stripper tower bottom.
Preferably, step (1) feedstock oil is coal tar fraction, preferably fraction of the coal tar at 250-420 DEG C, example
It such as can be 250 DEG C, 260 DEG C, 270 DEG C, 280 DEG C, 290 DEG C, 300 DEG C, 310 DEG C, 320 DEG C, 330 DEG C, 340 DEG C, 350 DEG C, 360
DEG C, 370 DEG C, 380 DEG C, 390 DEG C, 400 DEG C, 410 DEG C or fraction at 420 DEG C, preferably 300-350 DEG C of fraction.
Preferably, step (1) feedstock oil and the mixed temperature of hydrogen are 150-300 DEG C, such as can be 150
℃、160℃、170℃、180℃、190℃、200℃、210℃、220℃、230℃、240℃、250℃、260℃、270℃、
280 DEG C, 290 DEG C or 300 DEG C, preferably 200-250 DEG C.
Preferably, the volume ratio of the hydrogen and feedstock oil is (1000-3000): 1, such as can be 1000:1,1500:
1,2000:1,2500:1 or 3000:1, preferably (1500-3000): 1.
Preferably, the temperature of step (1) described hydrogenation reaction is 180-380 DEG C, such as can be 180 DEG C, 190 DEG C, 200
℃、210℃、220℃、230℃、240℃、250℃、260℃、270℃、280℃、290℃、300℃、310℃、320℃、
330 DEG C, 340 DEG C, 350 DEG C, 360 DEG C, 370 DEG C or 380 DEG C, preferably 200-380 DEG C.
Preferably, the pressure of the hydrogenation reaction be 12-20MPa, such as can be 12MPa, 13MPa, 14MPa,
15MPa, 16MPa, 17MPa, 18MPa, 19MPa or 20MPa, preferably 12-18MPa.
Preferably, the liquid hourly space velocity (LHSV) of the hydrogenation reaction is 0.2-1.2h-1, such as can be 0.2h-1、0.3h-1、0.4h-1、0.5h-1、0.6h-1、0.7h-1、0.8h-1、0.9h-1、1h-1、1.1h-1Or 1.2h-1, preferably 0.2-1.0h-1。
Hydrogenation catalyst used therein is the common catalyst of those skilled in the art when hydrogenation reaction of the present invention, such as be can be
The catalyst of platiniferous, palladium and nickel is not repeating herein, and those skilled in the art can reasonably be selected according to process requirement
It selects.
Preferably, the pressure of step (1) described gas-liquid separation be 10-18MPa, such as can be 10MPa, 11MPa,
12MPa, 13MPa, 14MPa, 15MPa, 16MPa, 17MPa or 18MPa, preferably 10-16MPa.
Preferably, the temperature of the gas-liquid separation is 250-300 DEG C, such as can be 250 DEG C, 260 DEG C, 270 DEG C, 280
DEG C, 290 DEG C or 300 DEG C, preferably 260-290 DEG C.
Preferably, the pressure of step (2) described fractionation be 0.1-0.5MPa, such as can be 0.1MPa, 0.15MPa,
0.2MPa, 0.25MPa, 0.3MPa, 0.35MPa, 0.4MPa, 0.45MPa or 0.5MPa, preferably 0.25-0.35MPa.
Preferably, the temperature of the fractionation be 250-300 DEG C, such as can be 250 DEG C, 260 DEG C, 270 DEG C, 280 DEG C,
290 DEG C or 300 DEG C, preferably 260-290 DEG C.
Preferably, step (3) stripping is to be stripped using superheated steam.
Preferably, the temperature of the superheated steam is 300-400 DEG C, such as can be 300 DEG C, 310 DEG C, 320 DEG C, 330
DEG C, 340 DEG C, 350 DEG C, 360 DEG C, 370 DEG C, 380 DEG C, 390 DEG C or 400 DEG C, preferably 330-360 DEG C.
Preferably, the flow of the superheated steam is 200-2000Kg/h, for example, can be 200,500,1000,
1500Kg/h or 2000Kg/h, preferably 400-1000Kg/h.
Preferably, the step of recycling the hydrogen in gas obtained by gas-liquid separation afterwards the method also includes step (1): gas
Gas-liquid separation is carried out after cooling, is mixed after the hydrogen obtained after gas-liquid separation is heated with the feedstock oil in step (1).
Water phase, light oil phase and fixed gas are generated after gas cooling, wherein fixed gas is hydrogen.
Preferably, the temperature after gas cooling is 45-55 DEG C, for example, can be 45 DEG C, 48 DEG C, 50 DEG C, 52 DEG C or
55℃。
Preferably, the pressure of the gas-liquid separation be 2-4MPa, such as can be 2MPa, 2.5MPa, 3MPa, 3.5MPa or
4MPa, preferably 2.5-3.5MPa.
Preferably, the temperature of the gas-liquid separation is 250-300 DEG C, such as can be 250 DEG C, 260 DEG C, 270 DEG C, 280
DEG C, 290 DEG C or 300 DEG C, preferably 260-290 DEG C.
As the optimal technical scheme of second aspect of the present invention providing method, described method includes following steps:
(1) it is mixed after feedstock oil heating with the hydrogen after heating, mixed temperature is 150-300 DEG C, hydrogen and raw material
The volume ratio of oil is (1000-3000): 1,180-380 DEG C, carry out hydrogenation reaction, the liquid hourly space velocity (LHSV) of hydrogenation reaction under 12-20MPa
For 0.2-1.2h-1, the gas-liquid separation under conditions of 10-18MPa, 250-300 DEG C after hydrogenation reaction, liquid phase is plus hydrogen base oil gas
The gas-liquid separation under conditions of 2-4MPa, 250-300 DEG C after being mutually cooled to 45-55 DEG C, obtain hydrogen heating after with feedstock oil
Mixing；
(2) fractionation plus hydrogen base oil under conditions of 0.1-0.5MPa, 250-300 DEG C, base oil light component is by the stripper
Portion's charging, base oil heavy constituent is by charging in the middle part of the stripper；
(3) it is using 300-400 DEG C of superheated steam stripping base oil light component and base oil heavy constituent, the flow of superheated steam
200-2000Kg/h obtains hydrogen supply dissolvent in stripper tower bottom.
Compared with the existing technology, the invention has the following advantages:
(1) hydrogen supply dissolvent provided by the invention for hydrogen index (HI) up to 20.82, hydrogen supply capacity is strong；
(2) process units structure provided by the invention is simple, and the utilization rate of hydrogen is high, and equipment investment is low, adds hydrogen solvent
Production cost it is low；
(3) process flow of hydrogen supply dissolvent preparation method provided by the invention is simple, passes through control hydrogen-oil ratio, reaction temperature
The operating parameters such as degree, reaction pressure, air speed, it is therefore prevented that the yield of the supersaturation of hydrogen supply dissolvent, hydrogen supply dissolvent is up to 88.64%.
Detailed description of the invention
Fig. 1 is the schematic diagram of the device for the production hydrogen supply dissolvent that the embodiment of the present invention 1 provides；
Fig. 2 is the schematic diagram of the device for the production hydrogen supply dissolvent that the embodiment of the present invention 2 provides；
Fig. 3 is the schematic diagram at the device for producing hydrogen supply dissolvent that the embodiment of the present invention 3 provides.
Wherein: 1, raw material oil tank；2, hydrogen heating furnace；3, feedstock oil delivery pump；4, heat exchanger；5, fixed bed reaction
Device；6, high pressure hot separator；7, thermal low-pressure separators；8, stripper；9, stripper return tank；10, air cooler；11, gas-liquid point
From device；12, compressor.
Specific embodiment
The technical scheme of the invention is further explained by means of specific implementation.Those skilled in the art should be bright
, the described embodiments are merely helpful in understanding the present invention, should not be regarded as a specific limitation of the invention.
Embodiment 1
A kind of device for producing hydrogen supply dissolvent is present embodiments provided, the schematic diagram of described device is as shown in Figure 1, include supplying
Hydrogen unit, feedstock oil feed unit, hydrogenation reaction unit, separative unit and stripper 8.
The feedstock oil feed unit includes sequentially connected raw material oil tank 1, feedstock oil delivery pump 3, heat exchanger 4；
The hydrogen supply unit includes hydrogen heating furnace 2, the outlet of the hydrogen heating furnace 2 and the entrance of hydrogenation reaction unit
It is connected, the connecting line between hydrogen heating furnace 2 and hydrogenation reaction unit entrance is also connected with the outlet of the heat exchanger 4；
The separative unit includes high pressure hot separator 6 and thermal low-pressure separators 7, and the high pressure hot separator 6 is provided with
Top gas outlet and the first bottom discharge port, the first bottom discharge port are connect with the entrance of the thermal low-pressure separators 7；The heat
Low pressure separator 7 is provided with top discharge mouth and the second bottom discharge port, the top discharge mouth and the second bottom discharge port point
It is not connect with the stripper 8 independently；
The hydrogenation reaction unit includes two fixed bed reactors 5, is connected in series between the fixed bed reactors 5,
The outlet of the last one fixed bed reactors 5 is connect after the heat exchanger 4 with the entrance of the high pressure hot separator 6.
Feedstock oil in raw material oil tank 1 flows through heat exchanger 4 under the action of feedstock oil delivery pump 3, after the heating with hydrogen
The hydrogen mixing that gas heating furnace 2 flows out, and enter in fixed bed reactors 5 reacted together, high temperature after reaction is mixed
It closes logistics to be used to heat feedstock oil through heat exchanger 4, the gas-liquid separation in high pressure hot separator 6 of the hot mixture after cooling, gas
Body is discharged by top gas outlet, adds hydrogen base oil to flow into thermal low-pressure separators 7 by the first bottom discharge port, and in thermal low-pressure separators
Fractionation is base oil light component and base oil heavy constituent in 7, wherein base oil light component is fed by 8 top of stripper, base oil heavy constituent by
It is fed in the middle part of stripper 8,8 bottom of stripper is passed through superheated steam for stripping base oil light component and base oil heavy constituent, and in vapour
8 bottom of stripper obtains plus hydrogen solvent.
Embodiment 2
A kind of device for producing hydrogen supply dissolvent is present embodiments provided, the schematic diagram of described device is as shown in Fig. 2, except stripping
It is additionally provided at the top of tower 8 outside stripper return tank 9, remaining is same as Example 1.
Feedstock oil in raw material oil tank 1 flows through heat exchanger 4 under the action of feedstock oil delivery pump 3, after the heating with hydrogen
The hydrogen mixing that gas heating furnace 2 flows out, and enter in fixed bed reactors 5 reacted together, high temperature after reaction is mixed
It closes logistics to be used to heat feedstock oil through heat exchanger 4, the gas-liquid separation in high pressure hot separator 6 of the hot mixture after cooling, gas
Body is discharged by top gas outlet, adds hydrogen base oil to flow into thermal low-pressure separators 7 by the first bottom discharge port, and in thermal low-pressure separators
Fractionation is base oil light component and base oil heavy constituent in 7, wherein base oil light component is fed by 8 top of stripper, base oil heavy constituent by
It is fed in the middle part of stripper 8,8 bottom of stripper is passed through superheated steam for stripping base oil light component and base oil heavy constituent, and in vapour
8 bottom of stripper obtains plus hydrogen solvent.
8 top gas phase of stripper flows into stripper return tank 9 and the gas-liquid separation in stripper return tank 9, fixed gas by
It is discharged at the top of stripper return tank 9, water phase is flowed out by 9 bottom of stripper return tank, and light oil phase a part is back to stripper 8
Top adds the yield of hydrogen solvent to improve, and another part is mutually exported discharge by light oil.
Embodiment 3
A kind of device for producing hydrogen supply dissolvent is present embodiments provided, the schematic diagram of described device is as shown in figure 3, with implementation
Example 2 is compared, and hydrogen recovery unit is additionally provided in the device that embodiment 3 provides, and the hydrogen recovery unit includes being sequentially connected
Air cooler 10, gas-liquid separator 11 and compressor 12, the top of the entrance of the air cooler 10 and the high pressure hot separator 6
The connection of portion gas outlet, the gas vent of the compressor 12 are connect with the entrance of hydrogen heating furnace 2, the gas-liquid separator 11
The water phase of water phase outlet and the stripper return tank 9, which exports, to be connected, and light oil mutually exports light with the stripper return tank 9
The mutually outlet connection of matter oil.
Feedstock oil in raw material oil tank 1 flows through heat exchanger 4 under the action of feedstock oil delivery pump 3, after the heating with hydrogen
The hydrogen mixing that gas heating furnace 2 flows out, and enter in fixed bed reactors 5 reacted together, high temperature after reaction is mixed
It closes logistics to be used to heat feedstock oil through heat exchanger 4, the gas-liquid separation in high pressure hot separator 6 of the hot mixture after cooling, gas
Body is discharged by top gas outlet, adds hydrogen base oil to flow into thermal low-pressure separators 7 by the first bottom discharge port, and in thermal low-pressure separators
Fractionation is base oil light component and base oil heavy constituent in 7, wherein base oil light component is fed by 8 top of stripper, base oil heavy constituent by
It is fed in the middle part of stripper 8,8 bottom of stripper is passed through superheated steam for stripping base oil light component and base oil heavy constituent, and in vapour
8 bottom of stripper obtains plus hydrogen solvent.
Enter gas-liquid separator 11 after the cooling of air cooler 10 by the gas of 6 top gas outlet of high pressure hot separator discharge,
And it is divided into fixed gas, water phase and light oil phase in gas-liquid separator 11, fixed gas enters hydrogen after the compression of compressor 12
Heating furnace 2 is heated, and is then mixed with feedstock oil, and water phase is discharged after mixing with the water phase that stripper return tank 9 flows out, lightweight
The oily light oil mutually flowed out with stripper return tank 9 is discharged after mixing.
8 top gas phase of stripper flows into stripper return tank 9 and the gas-liquid separation in stripper return tank 9, fixed gas by
It is discharged at the top of stripper return tank 9, water phase is flowed out by 9 bottom of stripper return tank, and light oil phase a part is back to stripper 8
Top adds the yield of hydrogen solvent to improve, and another part is mutually exported discharge by light oil.
Comparative example 1
This comparative example provides a kind of device for producing hydrogen supply dissolvent, compared with Example 3, the device that comparative example 1 provides
In be not provided with separative unit and hydrogen recovery unit, the outlet of the last one fixed bed reactors 5 is after the heat exchanger 4
It is connect with the middle part of stripper 8.
Feedstock oil in raw material oil tank 1 flows through heat exchanger 4 under the action of feedstock oil delivery pump 3, after the heating with hydrogen
The hydrogen mixing that gas heating furnace 2 flows out, and enter in fixed bed reactors 5 reacted together, high temperature after reaction is mixed
Logistics is closed through heat exchanger 4 for heating feedstock oil, the hot mixture after cooling in the middle part of stripper 8 by feeding, 8 bottom of stripper
Superheated steam is passed through for stripping base oil light component and base oil heavy constituent, and obtains adding hydrogen solvent in 8 bottom of stripper.
8 top gas phase of stripper flows into stripper return tank 9 and the gas-liquid separation in stripper return tank 9, fixed gas by
It is discharged at the top of stripper return tank 9, water phase is flowed out by 9 bottom of stripper return tank, and light oil phase a part is back to stripper 8
Top adds the yield of hydrogen solvent to improve, and another part is mutually exported discharge by light oil.
By taking 300-350 DEG C of coal tar of fraction as an example, hydrogen supply dissolvent is prepared using it as feedstock oil, the aromatic carbon rate of feedstock oil is
50.0%, it is 13.25 for hydrogen index (HI).
Application examples 1
The device that the application example provides a kind of production hydrogen supply dissolvent that Application Example 3 provides prepares the side of hydrogen supply dissolvent
Method, described method includes following steps:
(1) mix after feedstock oil heating with the hydrogen after heating, mixed temperature is 220 DEG C, hydrogen and feedstock oil
Volume ratio is 2000:1, and 220 DEG C, carry out hydrogenation reaction under 16MPa, the liquid hourly space velocity (LHSV) of hydrogenation reaction is 0.6h-1, after hydrogenation reaction
The gas-liquid separation under conditions of 14MPa, 280 DEG C, liquid phase are after adding hydrogen base oil, gas phase to be cooled to 50 DEG C in 3MPa, 280 DEG C of item
Gas-liquid separation under part mixes after obtained hydrogen heating with feedstock oil；
(2) 0.3MPa, fractionation plus hydrogen base oil under conditions of 280 DEG C, base oil light component are fed by 8 top of stripper,
Base oil heavy constituent in the middle part of the stripper 8 by feeding；
(3) it is using 350 DEG C of superheated steam stripping base oil light component and base oil heavy constituent, the flow of superheated steam
700Kg/h obtains hydrogen supply dissolvent in 8 tower bottom of stripper.
Application examples 2
The device that the application example provides a kind of production hydrogen supply dissolvent that Application Example 3 provides prepares the side of hydrogen supply dissolvent
Method, described method includes following steps:
(1) mix after feedstock oil heating with the hydrogen after heating, mixed temperature is 250 DEG C, hydrogen and feedstock oil
Volume ratio is 2500:1, and 250 DEG C, carry out hydrogenation reaction under 18MPa, the liquid hourly space velocity (LHSV) of hydrogenation reaction is 1h-1, after hydrogenation reaction in
16MPa, gas-liquid separation under conditions of 290 DEG C, liquid phase be plus hydrogen base oil, gas phase be cooled to 52 DEG C after in 3.5MPa, 290 DEG C of item
Gas-liquid separation under part mixes after obtained hydrogen heating with feedstock oil；
(2) 0.35MPa, fractionation plus hydrogen base oil under conditions of 290 DEG C, base oil light component are fed by 8 top of stripper,
Base oil heavy constituent in the middle part of the stripper 8 by feeding；
(3) it is using 360 DEG C of superheated steam stripping base oil light component and base oil heavy constituent, the flow of superheated steam
1000Kg/h obtains hydrogen supply dissolvent in 8 tower bottom of stripper.
Application examples 3
The device that the application example provides a kind of production hydrogen supply dissolvent that Application Example 3 provides prepares the side of hydrogen supply dissolvent
Method, described method includes following steps:
(1) mix after feedstock oil heating with the hydrogen after heating, mixed temperature is 200 DEG C, hydrogen and feedstock oil
Volume ratio is 1500:1, and 200 DEG C, carry out hydrogenation reaction under 14MPa, the liquid hourly space velocity (LHSV) of hydrogenation reaction is 0.4h-1, after hydrogenation reaction
The gas-liquid separation under conditions of 12MPa, 260 DEG C, liquid phase are after adding hydrogen base oil, gas phase to be cooled to 48 DEG C in 2.2MPa, 260 DEG C
Under the conditions of gas-liquid separation, obtain hydrogen heating after mixed with feedstock oil；
(2) 0.25MPa, fractionation plus hydrogen base oil under conditions of 260 DEG C, base oil light component are fed by 8 top of stripper,
Base oil heavy constituent in the middle part of the stripper 8 by feeding；
(3) it is using 330 DEG C of superheated steam stripping base oil light component and base oil heavy constituent, the flow of superheated steam
400Kg/h obtains hydrogen supply dissolvent in 8 tower bottom of stripper.
Application examples 4
The device that the application example provides a kind of production hydrogen supply dissolvent that Application Example 3 provides prepares the side of hydrogen supply dissolvent
Method, described method includes following steps:
(1) mix after feedstock oil heating with the hydrogen after heating, mixed temperature is 300 DEG C, hydrogen and feedstock oil
Volume ratio is 3000:1, and 300 DEG C, carry out hydrogenation reaction under 20MPa, the liquid hourly space velocity (LHSV) of hydrogenation reaction is 1.2h-1, after hydrogenation reaction
The gas-liquid separation under conditions of 18MPa, 300 DEG C, liquid phase are after adding hydrogen base oil, gas phase to be cooled to 55 DEG C in 4MPa, 300 DEG C of item
Gas-liquid separation under part mixes after obtained hydrogen heating with feedstock oil；
(2) 0.5MPa, fractionation plus hydrogen base oil under conditions of 300 DEG C, base oil light component are fed by 8 top of stripper,
Base oil heavy constituent in the middle part of the stripper 8 by feeding；
(3) it is using 400 DEG C of superheated steam stripping base oil light component and base oil heavy constituent, the flow of superheated steam
2000Kg/h obtains hydrogen supply dissolvent in 8 tower bottom of stripper.
Application examples 5
The device that the application example provides a kind of production hydrogen supply dissolvent that Application Example 3 provides prepares the side of hydrogen supply dissolvent
Method, described method includes following steps:
(1) mix after feedstock oil heating with the hydrogen after heating, mixed temperature is 150 DEG C, hydrogen and feedstock oil
Volume ratio is 1000:1, and 150 DEG C, carry out hydrogenation reaction under 12MPa, the liquid hourly space velocity (LHSV) of hydrogenation reaction is 0.2h-1, after hydrogenation reaction
The gas-liquid separation under conditions of 10MPa, 250 DEG C, liquid phase are after adding hydrogen base oil, gas phase to be cooled to 45 DEG C in 2MPa, 250 DEG C of item
Gas-liquid separation under part mixes after obtained hydrogen heating with feedstock oil；
(2) 0.1MPa, fractionation plus hydrogen base oil under conditions of 250 DEG C, base oil light component are fed by 8 top of stripper,
Base oil heavy constituent in the middle part of the stripper 8 by feeding；
(3) it is using 300 DEG C of superheated steam stripping base oil light component and base oil heavy constituent, the flow of superheated steam
200Kg/h obtains hydrogen supply dissolvent in 8 tower bottom of stripper.
Compare application examples 1
The device that this comparison application examples provides a kind of production hydrogen supply dissolvent that Comparison study example 1 provides prepares hydrogen supply dissolvent
Method, described method includes following steps:
(I) mix after feedstock oil heating with the hydrogen after heating, mixed temperature is 220 DEG C, hydrogen and feedstock oil
Volume ratio is 2000:1, and 220 DEG C, carry out hydrogenation reaction under 16MPa, the liquid hourly space velocity (LHSV) of hydrogenation reaction is 0.6h-1, obtain adding hydrogen
Oil；
(II) hydrogenated oil is stripped using 350 DEG C of superheated steam, the flow of superheated steam is 700Kg/h, in stripper tower
Bottom obtains hydrogen supply dissolvent.
The obtained hydrogen supply dissolvent of application examples 1-5 and comparison application examples 1 is analyzed, the aromatic carbon of gained hydrogen supply dissolvent
Rate, hydrogen supply dissolvent yield with it is as shown in table 1 for hydrogen index (HI), wherein for hydrogen index (HI) be every 1g hydrogen supply dissolvent middle ring alkylaromatic hydrocarbon on ring
The mg number of β reactive hydrogens of alkyl.
Table 1
As shown in Table 1, by coal tar for 300-350 DEG C of fraction prepares hydrogen supply dissolvent for feedstock oil, feedstock oil
Aromatic carbon rate is 50.0%, is 13.25 for hydrogen index (HI), the device and the application application examples 1-5 provided using the embodiment of the present application 3
The hydrogen supply dissolvent that the method for offer is prepared for hydrogen index (HI) 20 or more, peak 20.82, and the receipts of hydrogen supply dissolvent
Rate is up to 88.64%.
It compares the device that Comparison study example 1 provides in application examples 1 and produces hydrogen supply dissolvent, the device and reality that comparative example 1 provides
The device for applying the offer of example 3 is compared, and is not provided with separative unit and hydrogen recovery unit, the outlet of the last one fixed bed reactors
It is connect after heat exchanger with the middle part of stripper.Due to lacking hydrogen recovery unit, hydrogen can not sufficiently divide with hydrogen base oil is added
From adding hydrogen supersaturated, the aromatic carbon rate of gained hydrogen supply dissolvent is down to 38.2%, although the yield of the hydrogen supply dissolvent finally obtained is up to
90.37%, but also only have 17.63 for hydrogen index (HI), hydrogen supply effect is undesirable when using as hydrogen supply dissolvent.
In conclusion hydrogen supply dissolvent of the present invention is up to 20.82 for hydrogen index (HI), hydrogen supply capacity is strong；The hydrogen supply is molten
The process flow of agent preparation method is simple, by operating parameters such as control hydrogen-oil ratio, reaction temperature, reaction pressure, air speeds, prevents
The supersaturation of hydrogen supply dissolvent, and the yield of hydrogen supply dissolvent is up to 88.64%.
The Applicant declares that the foregoing is merely a specific embodiment of the invention, but protection scope of the present invention not office
It is limited to this, it should be clear to those skilled in the art, any to belong to those skilled in the art and take off in the present invention
In the technical scope of dew, any changes or substitutions that can be easily thought of, and all of which fall within the scope of protection and disclosure of the present invention.
Claims (10)
1. a kind of device for producing hydrogen supply dissolvent, which is characterized in that described device include hydrogen supply unit, feedstock oil feed unit,
Hydrogenation reaction unit, separative unit and stripper；
The feedstock oil feed unit includes sequentially connected raw material oil tank, feedstock oil delivery pump, heat exchanger；
The hydrogen supply unit includes hydrogen heating furnace, and the outlet of the hydrogen heating furnace is connected with the entrance of hydrogenation reaction unit,
Connecting line between hydrogen heating furnace and hydrogenation reaction unit entrance is also connected with the outlet of the heat exchanger；
The separative unit includes the first separator and the second separator, and first separator is provided with top gas outlet and the
One bottom discharge port, the first bottom discharge port are connect with the entrance of second separator；Second separator is provided with top
Portion's discharge port and the second bottom discharge port, the top discharge mouth and the second bottom discharge port separately with the stripper
Connection；
The hydrogenation reaction unit includes at least one hydrogenator, is connected in series between the hydrogenator, last
The outlet of a hydrogenator is connect after the heat exchanger with the entrance of first separator.
2. the apparatus according to claim 1, which is characterized in that the hydrogenation reaction unit includes 2-5 hydrogenator,
Preferably 2 hydrogenators；
Preferably, the hydrogenator is fixed bed reactors；
Preferably, first separator is high pressure hot separator；
Preferably, second separator is thermal low-pressure separators；
Preferably, the stripper top is additionally provided with stripper return tank.
3. device according to claim 1 or 2, which is characterized in that described device is additionally provided with hydrogen recovery unit, described
Hydrogen recovery unit includes sequentially connected air cooler, gas-liquid separator and compressor, the entrance of the air cooler with it is described
The top gas outlet of first separator connects, and the gas vent of the compressor is connect with the entrance of hydrogen heating furnace；
Preferably, the water phase outlet of the gas-liquid separator and the water phase of the stripper return tank are exported and are connected；
Preferably, the light oil of the gas-liquid separator is mutually exported mutually to export with the light oil of the stripper return tank and be connect.
4. a kind of method for preparing hydrogen supply dissolvent using the described in any item devices of claim 1-3, which is characterized in that the side
Method includes the following steps:
(1) feedstock oil and hydrogen after Hybrid Heating, gas-liquid separation after hydrogenation reaction obtain plus hydrogen base oil；
(2) fractionation plus hydrogen base oil, base oil light component are fed by the stripper top, and base oil heavy constituent is by the stripper middle part
Charging；
(3) stripping base oil light component and base oil heavy constituent obtain hydrogen supply dissolvent oil in stripper tower bottom.
5. according to the method described in claim 4, it is characterized in that, step (1) feedstock oil is coal tar fraction；
Preferably, the coal tar fraction is fraction of the coal tar at 250-420 DEG C, preferably 300-350 DEG C of fraction；
Preferably, step (1) feedstock oil and the mixed temperature of hydrogen are 150-300 DEG C, preferably 200-250 DEG C；
Preferably, the volume ratio of the hydrogen and feedstock oil is (1000-3000): 1, preferably (1500-3000): 1；
Preferably, the temperature of the hydrogenation reaction is 180-380 DEG C, preferably 200-380 DEG C；
Preferably, the pressure of the hydrogenation reaction is 12-20MPa, preferably 12-18MPa；
Preferably, the liquid hourly space velocity (LHSV) of the hydrogenation reaction is 0.2-1.2h-1, preferably 0.2-1.0h-1。
6. method according to claim 4 or 5, which is characterized in that the pressure of step (1) described gas-liquid separation is 10-
18MPa, preferably 10-16MPa；
Preferably, the temperature of the gas-liquid separation is 250-300 DEG C, preferably 260-290 DEG C.
7. according to the described in any item methods of claim 4-6, which is characterized in that the pressure of step (2) described fractionation is 0.1-
0.5MPa, preferably 0.25-0.35MPa；
Preferably, the temperature of the fractionation is 250-300 DEG C, preferably 260-290 DEG C.
8. according to the described in any item methods of claim 4-7, which is characterized in that step (3) stripping steams to use to overheat
Vapour stripping；
Preferably, the temperature of the superheated steam is 300-400 DEG C, preferably 330-360 DEG C；
Preferably, the flow of the superheated steam is 200-2000Kg/h, preferably 400-1000Kg/h.
9. according to the described in any item methods of claim 4-8, which is characterized in that the method also includes steps (1) to recycle afterwards
The step of hydrogen in gas obtained by gas-liquid separation: gas-liquid separation is carried out after gas cooling, the hydrogen warp obtained after gas-liquid separation
It is mixed after heating with the feedstock oil in step (1)；
Preferably, the temperature after the gas cooling is 45-55 DEG C；
Preferably, the pressure of the gas-liquid separation is 2-4MPa, preferably 2.5-3.5MPa；
Preferably, the temperature of the gas-liquid separation is 250-300 DEG C, preferably 260-290 DEG C.
10. according to the described in any item methods of claim 4-9, which is characterized in that described method includes following steps:
(1) mix after feedstock oil heating with the hydrogen after heating, mixed temperature is 150-300 DEG C, hydrogen and feedstock oil
Volume ratio is (1000-3000): 1,180-380 DEG C, carry out hydrogenation reaction under 12-20MPa, the liquid hourly space velocity (LHSV) of hydrogenation reaction is
0.2-1.2h-1, the gas-liquid separation under conditions of 10-18MPa, 250-300 DEG C after hydrogenation reaction, liquid phase is plus hydrogen base oil gas phase
The gas-liquid separation under conditions of 2-4MPa, 250-300 DEG C after being cooled to 45-55 DEG C, it is mixed with feedstock oil after obtained hydrogen heating
It closes；
(2) fractionation plus hydrogen base oil under conditions of 0.1-0.5MPa, 250-300 DEG C, base oil light component by the stripper top into
Material, base oil heavy constituent is by charging in the middle part of the stripper；
(3) using 300-400 DEG C of superheated steam stripping base oil light component and base oil heavy constituent, the flow of superheated steam is 200-
2000Kg/h obtains hydrogen supply dissolvent in stripper tower bottom.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1865399A (en) * | 2006-06-09 | 2006-11-22 | 神华集团有限责任公司 | Preparation method of initiating solvent for direct liquefy of coal |
| US20140275691A1 (en) * | 2013-03-15 | 2014-09-18 | Butts Properties, Ltd. | System and Method for H2S Removal Integrated with Stinson Process CO2 Removal |
| CN108264933A (en) * | 2016-12-30 | 2018-07-10 | 北京华石联合能源科技发展有限公司 | A kind of device that heavy oil lighting is realized using floating bed hydrogenation technology |
-
2019
- 2019-05-08 CN CN201910380736.9A patent/CN110003949B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1865399A (en) * | 2006-06-09 | 2006-11-22 | 神华集团有限责任公司 | Preparation method of initiating solvent for direct liquefy of coal |
| US20140275691A1 (en) * | 2013-03-15 | 2014-09-18 | Butts Properties, Ltd. | System and Method for H2S Removal Integrated with Stinson Process CO2 Removal |
| CN108264933A (en) * | 2016-12-30 | 2018-07-10 | 北京华石联合能源科技发展有限公司 | A kind of device that heavy oil lighting is realized using floating bed hydrogenation technology |
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