CN108003929A - A kind of heavy benzene hydrogenation process for refining - Google Patents

A kind of heavy benzene hydrogenation process for refining Download PDF

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Publication number
CN108003929A
CN108003929A CN201711361392.4A CN201711361392A CN108003929A CN 108003929 A CN108003929 A CN 108003929A CN 201711361392 A CN201711361392 A CN 201711361392A CN 108003929 A CN108003929 A CN 108003929A
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benzene
hydrogenation reactor
heavy
hydrogenation
hydrogen
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CN201711361392.4A
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金冬梅
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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
    • 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
    • C10G2400/02—Gasoline
    • 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

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  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)

Abstract

The present invention relates to a kind of heavy benzene hydrogenation process for refining, heavy benzol and hydrogen are separately added into the first hydrogenation reactor and carry out pre-hydrotreating reaction by the technique, reaction product enters de- benzene unit, isolate benzene, toluene and dimethylbenzene, remaining ingredient is sent into evaporator and is vaporized, and after the boil-off gas of evaporator outlet is mixed with hydrogen, hydrofining reaction is carried out into the second hydrogenation reactor, reaction product carries out rectifying separation again, respectively obtains gasoline fraction and diesel oil distillate.The heavy benzene hydrogenation process for refining of the present invention directly can carry out hydrotreating by counterweight benzene raw materials, promote the further utilization of coal tar, and capacity usage ratio is high, superior product quality, catalyst life length.

Description

A kind of heavy benzene hydrogenation process for refining
Technical field
The present invention relates to technical field of petrochemical industry, more particularly to a kind of heavy benzene hydrogenation process for refining.
Background technology
Heavy benzol is the accessory substance produced during crude benzole hydrogenation, to be colourless to pale yellow oily liquid, there is similar chloroform Smell, density 0.960-0.990g/cm3 is not soluble in water, volatile, inflammable, poisonous, can be most organic with benzene, ketone, ester, alcohol etc. Solvent is miscible.In crude benzole hydrogenation technical process, raw material crude benzol is separated in multi-stage evaporation device, high boiling component such as front three Benzene, naphthalene, indane, coumarone etc. are discharged as Residual oil from multi-stage evaporation device bottom, this part Residual oil is heavy benzol.
Most domestic producer is all used for heavy benzol as raw fuel stock or solvent oil processing, only only a few enterprise at present Coumarone-indene resin is produced, because Petropols are more more competitive than coumarone indene resin in price and performance etc., and it is ancient The grand resin toxic of horse, is progressively substituted by Petropols.Further, since contain the heterocyclic compounds such as a certain amount of O, S, N in heavy benzol Thing, also has penetrating odor as solvent naphtha except stability difference is outer, and not only quality is not high during directly as fuel oil and pollution Environment, i.e., at present these purposes there are poor product quality, lack competitiveness or pollute environment the problem of.Therefore, it is necessary to plus Strong heavy benzene hydrogenation purification techniques, the new utilization ways of exploitation heavy benzol extend coal-coking-Fine Chemical Industry chain, and increase product is attached It is value added.
The content of the invention
, can it is an object of the present invention to provide a kind of heavy benzene hydrogenation process for refining for the above problem of the prior art Direct counterweight benzene raw materials carry out hydrotreating, promote the further utilization of coal tar.
To solve the above-mentioned problems, technical scheme is as follows：
A kind of heavy benzene hydrogenation process for refining, heavy benzol and hydrogen are separately added into the first hydrogenation reactor and carry out pre-hydrotreating reaction, Reaction product enters de- benzene unit, isolates benzene, toluene and dimethylbenzene, and remaining ingredient is sent into evaporator and is vaporized, and evaporates After the boil-off gas of device outlet is mixed with hydrogen, carry out hydrofining reaction into the second hydrogenation reactor, reaction product again into Row rectifying separates, and respectively obtains gasoline fraction and diesel oil distillate, wherein,
The operating condition of first hydrogenation reactor is：Pressure 8-12MPa, 120-200 DEG C of temperature, volume space velocity degree 0.5-6/ H, hydrogen to oil volume ratio 100-500:1；
The operating condition of second hydrogenation reactor is：Pressure 8-12MPa, 300-350 DEG C of temperature, volume space velocity 0.3-0.8/ H, hydrogen to oil volume ratio 500-1000:1.
Further, the first catalyst bed is equipped with first hydrogenation reactor, first catalyst bed Catalyst is using Pd as active component, and Mo is auxiliary agent, γ-Al2O3For carrier, wherein, the load capacity of active component Pd is 3%-8%, Mo Load capacity be 1%-3%, and the weight ratio of Pd and Mo is 2:1~4:1.
Further, the second catalyst bed is equipped with second hydrogenation reactor, second catalyst bed Catalyst is with W2N active components, Fe are auxiliary agent, γ-Al2O3For carrier, wherein, active component W2The load capacity of N is 6% ~ 13%, The load capacity of auxiliary agent Fe is 0.5% ~ 5%, and W2The weight ratio of N and Fe is 1.5:1~5:1.
Further, the gasoline that the benzene,toluene,xylene that the de- benzene unit is isolated is isolated with the rectifying is evaporated Gasoline products are used as after split-phase mixing.
Further, recuperation of heat range site, the diesel oil that the rectifying is isolated are equipped with before first hydrogenation reactor Cut heats the heavy benzol for entering first hydrogenation reactor in the recuperation of heat range site.
A kind of heavy benzene hydrogenation process for refining of the present invention, has the advantages that：
（1）The present invention directly carries out hydrogenation reaction by raw material of heavy benzol, and without carrying out separating treatment to raw material, technique is simple, easily In control.
（2）The first hydrogenation reactor of the present invention carries out hydrotreating to the alkene in heavy benzol, can prevent subsequent process The polymerism of middle generation, extends the service life of catalyst.
（3）The present invention by benzene, toluene and dimethylbenzene, was reacted in de- benzene unit so as to reduce the second hydrogenation reactor Hydrogen consumption in journey, adds the octane number of gasoline fraction.
（4）The remaining ingredient of de- benzene unit is first sent into evaporator vaporization by the present invention, and after boil-off gas is mixed with hydrogen The second hydrogenation reactor is re-fed into, due to being homogeneous reaction in the second hydrogenation reactor（It is gas phase）, so as to greatly improve The yield of product, reduces reaction temperature.Further, since the boil-off gas temperature of evaporator outlet has reached the second hydrogenation reaction Reaction temperature in device, so as to save the step of being heated to the raw material for entering the second hydrogenation reactor, reduces and is The overall energy consumption of system, capacity usage ratio is high, and superior product quality, simplifies technique.
（5）The present invention is equipped with recuperation of heat range site before the first hydrogenation reactor, sufficiently make use of rectifying to isolate Diesel oil distillate heat, improve capacity usage ratio.
Brief description of the drawings
, below will be to required in embodiment or description of the prior art in order to illustrate more clearly of technical scheme The attached drawing used is briefly described.It should be evident that drawings in the following description are only some embodiments of the present invention, it is right For those of ordinary skill in the art, without creative efforts, it can also be obtained according to these attached drawings Its attached drawing.
Fig. 1 is a kind of FB(flow block) of heavy benzene hydrogenation process for refining provided by the invention；
In figure：The first hydrogenation reactors of 1-, 2- take off benzene unit, and 3- evaporators, the second hydrogenation reactors of 4-, 5- recuperations of heat utilize single Member.
Embodiment
Below in conjunction with the attached drawing in the embodiment of the present invention, the technical solution in the embodiment of the present invention is carried out clear, complete Site preparation describes, it is clear that described embodiment is only part of the embodiment of the present invention, instead of all the embodiments.It is based on Embodiment in the present invention, those of ordinary skill in the art obtained on the premise of creative work is not made it is all its His embodiment, belongs to the scope of protection of the invention.
The present invention provides a kind of heavy benzene hydrogenation process for refining, as shown in Figure 1, heavy benzol and hydrogen are separately added into the first hydrogenation Pre-hydrotreating reaction is carried out in reactor 1, reaction product enters de- benzene unit 2, isolates benzene, toluene and dimethylbenzene, remaining ingredient Be sent into evaporator 3 in be vaporized, evaporator 3 export boil-off gas mixed with hydrogen after, into the second hydrogenation reactor 4 into Row hydrofining reaction, reaction product carry out rectifying separation, respectively obtain gasoline fraction and diesel oil distillate again.The gasoline fraction with Gasoline products are used as after the benzene,toluene,xylene mixing that de- benzene unit 2 is isolated.Heat is equipped with before the first hydrogenation reactor 1 Unit 5 is recycled, the diesel oil distillate that the rectifying is isolated is in the recuperation of heat range site 5 to entering the described first hydrogenation The heavy benzol of reactor 1 is heated.
Wherein, the operating condition of first hydrogenation reactor 1 is：Pressure 8-12MPa, 120-200 DEG C of temperature, volume are empty Speed 0.5-6/h, hydrogen to oil volume ratio 100-500:1；The operating condition of second hydrogenation reactor 4 is：Pressure 8-12MPa, 300-350 DEG C of temperature, volume space velocity 0.3-0.8/h, hydrogen to oil volume ratio 500-1000:1.Set in first hydrogenation reactor 1 There is the first catalyst bed, the catalyst of first catalyst bed is using Pd as active component, and Mo is auxiliary agent, γ-Al2O3For Carrier, wherein, the load capacity of active component Pd is 3%-8%, and the load capacity of Mo is 1%-3%, and the weight ratio of Pd and Mo is 2:1~ 4:1.The second catalyst bed is equipped with second hydrogenation reactor 4, the catalyst of second catalyst bed is with W2N lives Property component, Fe is auxiliary agent, γ-Al2O3For carrier, wherein, active component W2The load capacity of N is 6% ~ 13%, the load capacity of auxiliary agent Fe For 0.5% ~ 5%, and W2The weight ratio of N and Fe is 1.5:1~5:1.
In order to further illustrate the heavy benzene hydrogenation process for refining of the present invention, illustrated below with specific embodiment, certainly The present invention and from the limitation of the following example.
Embodiment 1
First catalyst bed is set in the first hydrogenation reactor, and the catalyst of first catalyst bed is：3%Pd-1%Mo/ γ-Al2O3.Second catalyst bed is set in the second hydrogenation reactor, and the catalyst of second catalyst bed is：6%W2N- 0.7%Fe/γ-Al2O3。
The operating condition of first hydrogenation reactor is：Pressure 8MPa, 120 DEG C of temperature, volume space velocity degree 2/h, hydrogen oil volume Than 200:1.The operating condition of second hydrogenation reactor is：Pressure 8MPa, 300 DEG C, volume space velocity 0.3/h of temperature, hydrogen oil volume Than 600:1.Evaporator outlet temperature is 320 DEG C.
After testing, after hydrogenation reaction, the sulfur contents of gasoline products is 22ppm, nitrogen content 25ppm, and oxygen content is 15ppm, the octane number of gasoline products reach 98.The sulfur content of diesel product is 55ppm, nitrogen content 82ppm, and oxygen content is 17ppm, the Cetane number of diesel product reach 51.
Embodiment 2
First catalyst bed is set in the first hydrogenation reactor, and the catalyst of first catalyst bed is：5%Pd-2%Mo/ γ-Al2O3.Second catalyst bed is set in the second hydrogenation reactor, and the catalyst of second catalyst bed is：8%W2N- 2%Fe/γ-Al2O3。
The operating condition of first hydrogenation reactor is：Pressure 10MPa, 150 DEG C of temperature, volume space velocity degree 4/h, hydrogen oil volume Than 300:1.The operating condition of second hydrogenation reactor is：Pressure 10MPa, 330 DEG C, volume space velocity 0.5/h of temperature, hydrogen oil volume Than 800:1.Evaporator outlet temperature is 350 DEG C.
After testing, after hydrogenation reaction, the sulfur contents of gasoline products is 19ppm, nitrogen content 23ppm, and oxygen content is 13ppm, the octane number of gasoline products reach 98.5.The sulfur content of diesel product is 57ppm, nitrogen content 85ppm, and oxygen content is 15ppm, the Cetane number of diesel product reach 53.
Embodiment 3
First catalyst bed is set in the first hydrogenation reactor, and the catalyst of first catalyst bed is：8%Pd-2%Mo/ γ-Al2O3.Second catalyst bed is set in the second hydrogenation reactor, and the catalyst of second catalyst bed is：10%W2N- 4%Fe/γ-Al2O3。
The operating condition of first hydrogenation reactor is：Pressure 12MPa, 200 DEG C of temperature, volume space velocity degree 4/h, hydrogen oil volume Than 500:1.The operating condition of second hydrogenation reactor is：Pressure 12MPa, 350 DEG C, volume space velocity 0.8/h of temperature, hydrogen oil volume Than 1000:1.Evaporator outlet temperature is 350 DEG C.
After testing, after hydrogenation reaction, the sulfur contents of gasoline products is 28ppm, nitrogen content 29ppm, and oxygen content is 17ppm, the octane number of gasoline products reach 96.5.The sulfur content of diesel product is 52ppm, nitrogen content 81ppm, and oxygen content is 15ppm, the Cetane number of diesel product reach 49.
In summary, a kind of heavy benzene hydrogenation process for refining of the invention, has the advantages that：
（1）The present invention directly carries out hydrogenation reaction by raw material of heavy benzol, and without carrying out separating treatment to raw material, technique is simple, easily In control.
（2）The first hydrogenation reactor of the present invention carries out hydrotreating to the alkene in heavy benzol, can prevent subsequent process The polymerism of middle generation, extends the service life of catalyst.
（3）The present invention by benzene, toluene and dimethylbenzene, was reacted in de- benzene unit so as to reduce the second hydrogenation reactor Hydrogen consumption in journey, adds the octane number of gasoline fraction.
（4）The remaining ingredient of de- benzene unit is first sent into evaporator vaporization by the present invention, and after boil-off gas is mixed with hydrogen The second hydrogenation reactor is re-fed into, due to being homogeneous reaction in the second hydrogenation reactor（It is gas phase）, so as to greatly improve The yield of product, reduces reaction temperature.Further, since the boil-off gas temperature of evaporator outlet has reached the second hydrogenation reaction Reaction temperature in device, so as to save the step of being heated to the raw material for entering the second hydrogenation reactor, reduces and is The overall energy consumption of system, capacity usage ratio is high, and superior product quality, simplifies technique.
（5）The present invention is equipped with recuperation of heat range site before the first hydrogenation reactor, sufficiently make use of rectifying to isolate Diesel oil distillate heat, improve capacity usage ratio.
Described above has fully disclosed the embodiment of the present invention.It is pointed out that it is familiar with the field Scope of the technical staff to any change that the embodiment of the present invention is done all without departing from claims of the present invention. Correspondingly, the scope of claim of the invention is also not limited only to previous embodiment.

Claims (5)

  1. A kind of 1. heavy benzene hydrogenation process for refining, it is characterised in that by heavy benzol and hydrogen be separately added into the first hydrogenation reactor into Row pre-hydrotreating reaction, reaction product enter de- benzene unit, isolate benzene, toluene and dimethylbenzene, and remaining ingredient is sent into evaporator It is vaporized, after the boil-off gas of evaporator outlet is mixed with hydrogen, hydrofining reaction is carried out into the second hydrogenation reactor, Reaction product carries out rectifying separation again, respectively obtains gasoline fraction and diesel oil distillate, wherein,
    The operating condition of first hydrogenation reactor is：Pressure 8-12MPa, 120-200 DEG C of temperature, volume space velocity degree 0.5-6/ H, hydrogen to oil volume ratio 100-500:1；
    The operating condition of second hydrogenation reactor is：Pressure 8-12MPa, 300-350 DEG C of temperature, volume space velocity 0.3-0.8/ H, hydrogen to oil volume ratio 500-1000:1.
  2. 2. a kind of heavy benzene hydrogenation process for refining according to claim 1, it is characterised in that in first hydrogenation reactor Equipped with the first catalyst bed, the catalyst of first catalyst bed is using Pd as active component, and Mo is auxiliary agent, γ-Al2O3 For carrier, wherein, the load capacity of active component Pd is 3%-8%, and the load capacity of Mo is 1%-3%, and the weight ratio of Pd and Mo is 2:1 ~4:1。
  3. 3. a kind of heavy benzene hydrogenation process for refining according to claim 1, it is characterised in that in second hydrogenation reactor Equipped with the second catalyst bed, the catalyst of second catalyst bed is with W2N active components, Fe are auxiliary agent, γ-Al2O3For Carrier, wherein, active component W2The load capacity of N is 6% ~ 13%, and the load capacity of auxiliary agent Fe is 0.5% ~ 5%, and W2The weight of N and Fe Than for 1.5:1~5:1.
  4. 4. a kind of heavy benzene hydrogenation process for refining according to claim 1, it is characterised in that isolate the de- benzene unit The gasoline fraction isolated of benzene,toluene,xylene and the rectifying mix after be used as gasoline products.
  5. 5. a kind of heavy benzene hydrogenation process for refining according to claim 1, it is characterised in that before first hydrogenation reactor Equipped with recuperation of heat range site, the diesel oil distillate that the rectifying is isolated is in the recuperation of heat range site to entering described first The heavy benzol of hydrogenation reactor is heated.
CN201711361392.4A 2017-12-18 2017-12-18 A kind of heavy benzene hydrogenation process for refining Pending CN108003929A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102766007A (en) * 2012-08-15 2012-11-07 河南宝舜化工科技有限公司 Device and method for coked crude benzene full-fraction hydrofining and catalyst
CN104774648A (en) * 2015-03-18 2015-07-15 大连理工大学 Heavy benzol hydrofining method of clean fuel oil
CN205759793U (en) * 2016-05-27 2016-12-07 山东华鸿化工有限公司 A kind of Nitrobenzene Rectification system
CN107365241A (en) * 2017-06-28 2017-11-21 徐州东兴能源有限公司 A kind of crude benzole hydrogenation process for refining

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102766007A (en) * 2012-08-15 2012-11-07 河南宝舜化工科技有限公司 Device and method for coked crude benzene full-fraction hydrofining and catalyst
CN104774648A (en) * 2015-03-18 2015-07-15 大连理工大学 Heavy benzol hydrofining method of clean fuel oil
CN205759793U (en) * 2016-05-27 2016-12-07 山东华鸿化工有限公司 A kind of Nitrobenzene Rectification system
CN107365241A (en) * 2017-06-28 2017-11-21 徐州东兴能源有限公司 A kind of crude benzole hydrogenation process for refining

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Application publication date: 20180508