CN109988641A - Flexible hydrogenation of shale oil process - Google Patents
Flexible hydrogenation of shale oil process Download PDFInfo
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- CN109988641A CN109988641A CN201711469253.3A CN201711469253A CN109988641A CN 109988641 A CN109988641 A CN 109988641A CN 201711469253 A CN201711469253 A CN 201711469253A CN 109988641 A CN109988641 A CN 109988641A
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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
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/201—Impurities
- C10G2300/202—Heteroatoms content, i.e. S, N, O, P
-
- 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
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/30—Physical properties of feedstocks or products
- C10G2300/302—Viscosity
-
- 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
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/30—Physical properties of feedstocks or products
- C10G2300/304—Pour point, cloud point, cold flow properties
-
- 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 invention discloses a kind of flexible hydrogenation of shale oil process.Shale oil raw material carries out gas-liquid separation after weighted BMO spaces, and isolated liquid phase by being hydrocracked preatreating reactors, then proceedes to hydrocracking reactor, be divided into two strands by the material after the first hydrocracking catalyst bed first；Gas-liquid separator of one material through being arranged among bed obtains liquid phase, and extracts hydrocracking reactor out, enters hydroisomerizing cracker and carries out isocraking reaction；Material after extraction liquid phase continues to flow downwardly through the second hydrocracking catalyst bed；Institute's hydrocracking reaction material and hydroisomerizing cracking reaction material carry out gas-liquid separation and fractionation respectively, obtain different size, naphtha, boat coal, diesel oil and tail oil product.The present invention provide for the first time it is a kind of on a set of hydrogenation technique device and meanwhile produce two or more different size light naphthars, heavy naphtha, boat coal, diesel oil, tail oil product hydrocracking process.
Description
Technical field
The invention belongs to petroleum refining fields, and in particular to one kind flexibly produces of different nature using shale oil as feedstock oil
High-quality light naphthar, heavy naphtha, boat coal, diesel oil, tail oil product hydrocracking process.
Background technique
Hydrogen addition technology is the important manufacturing process of light materialization of heavy oil and light-end products quality upgrading.Hydrocracking technology because
Feedstock oil is adaptable, product flexibility is good, liquid product yield is high, high quality has obtained faster development.
Existing hydrocracking technology can be divided into three kinds according to processing flow: one-stage serial hydrocracking process flow, single hop add hydrogen
Process process and two-stage reforming process flow.According to tail oil, whether circulate operation can be divided into three kinds: one way is primary
Pass through process flow, part circulation technology process and complete alternation process flow.Inverted sequence hydrocracking technology is a kind of for raw material
Middle light fraction is more or the hydrocracking technology of the mostly equal exploitations of impurity (such as oxygen, metal) content.Hydrocracking technology uses two
The catalyst of seed type, pretreating catalyst by hydrocracking and hydrocracking catalyst, wherein hydrocracking catalyst is according to making
Different with Cracking Component can be divided into different types of catalyst again, and main Cracking Component includes amorphous silica-alumina, Y type
Molecular sieve, beta molecular sieve, SAPO Series Molecules sieve and ZSM-5 molecular sieve etc..A group timesharing, institute are hydrocracked using different type
Obtained light-end products composition and property also has biggish difference, and the composition and property of tail oil also have biggish difference.
CN101333459A discloses a kind of hydrogenating conversion process using inverted sequence hydrocracking process process, this method
It is suitble to the processing of long distillate feedstock oil；CN105733674A discloses a kind of inverted sequence method for hydrogen cracking, will mainly hydrogen be added to split
A part of gas phase extraction device of change process production, reduces the further cracking of small molecule material；CN103055922B is public
A kind of preparation method of body phase hydrocracking catalyst, CN105018139B, CN 001293228A, CN001508225A are opened
Two kinds are used with gradation in a kind of all disclosed method for hydrogen cracking of the high-output qulified industrial chemicals of low energy consumption of CN104611020B
The method of different Y type molecular sieves.Such technology can be hydrocracked using wax oil as feedstock oil by using containing Y type molecular sieve
The method for hydrogen cracking of catalyst yields products of quality, and wherein Determination of Alkane Content height, BMCI value are low in tail oil, is quality steam cracking
The raw material of ethylene processed, but the product for being hydrocracked each obtained fraction only has a kind of specification.
CN105582992A discloses a kind of hydroisomerisation catalysts and its preparation method and application and a kind of plus hydrogen
Cracking tail oil hydroisomerization process, such technology can using wax oil as feedstock oil, by using contain heterogeneous types molecular sieve
The method for hydrogen cracking of hydrocracking catalyst yields products of quality, and wherein isomery content height, condensation point are low in tail oil, viscosity index (VI)
Height, the product for being the raw material of High Quality Lube Base Oils, but being hydrocracked each obtained fraction only have a kind of specification.
CN103394368B discloses a kind of light oil type hydrogen cracking catalyst and preparation method thereof containing composite molecular screen
And application, CN103551186B disclose a kind of middle oil type hydrocracking catalyst containing composite molecular screen and preparation method thereof and
Using US4837396A discloses a kind of preparation of complex type molecular sieve catalysis.Such technology can using wax oil as feedstock oil,
By using the method for hydrogen cracking containing Y type molecular sieve and heterogeneous types molecular sieve complex type molecular sieve hydrocracking catalyst
Various high-quality hydrocracked products are produced, but the product of each fraction only has a kind of specification.
CN001169919C is disclosed a kind of to be raised productivity and improved the quality the method for diesel oil by distillate.Such technology can be with wax oil
Feedstock oil, while being catalyzed using containing Y zeolite catalyst and containing two kinds of heterogeneous types molecular sieve hydrocracking catalyst
The method for hydrogen cracking of agent produces various high-quality hydrocracked products, but the product of each fraction only has a kind of specification.
In conclusion the existing hydrocracking technology using two kinds of different type molecular sieve catalysts of comparison, uses Y type
The hydrocracking technology of molecular sieve hydrocracking catalyst, obtained heavy naphtha product sulfur content is low, virtue dive it is relatively high,
Navigating, product of coal smoke point is relatively high, and diesel product sulfur content is low, and Cetane number is high, but condensation point is relatively high, tail oil product virtue
Hydrocarbon content is low, and density is relatively small, and BMCI value is relatively low, but condensation point is very high, and typically larger than 30 DEG C；Use heterogeneous types
The hydrocracking technology of molecular sieve hydrocracking catalyst, obtained heavy naphtha product sulfur content is low, and virtue is latent relatively slightly lower,
Diesel product sulfur content is low, and condensation point is low, but Cetane number is relatively slightly lower, and tail oil density is relatively large, but isomery hydrocarbon content
Height, condensation point is very low, and usually less than 0 DEG C；Use the hydrocracking technology of the complex type molecular sieve catalysis of isomery containing Y-, Huo Zheji
Skill is hydrocracked with use hydrocracking catalyst containing Y type molecular sieve and the molecular sieve hydrocracking catalyst containing heterogeneous types
Art, obtained tail oil property is between using Y type molecular sieve hydrocracking catalyst and heterogeneous types molecular sieve is used to split
Change between catalyst.Above-mentioned hydrocracking process technology, the hydrocracking tail oil differentiation of product produced in identical conversion ratio
It is larger, wherein being the quality raw materials of preparing ethylene by steam cracking using the tail oil of Y zeolite catalyst, use heterogeneous types molecule
The tail oil of sieve catalyst is can directly to produce High Quality Lube Base Oils or the raw material as High Quality Lube Base Oils, is made
Using hydrocracking catalyst containing Y type molecular sieve and contain heterogeneous types with the complex type molecular sieve catalysis of isomery containing Y- or gradation
The tail oil that molecular sieve hydrocracking catalyst obtains can be used as the raw material of preparing ethylene by steam cracking or as high-quality lubricating oil
The raw material of base oil.When above-mentioned several hydrocracking process therefore are used alone, different types of add can only be selected as needed
Hydrogen Cracking catalyst is perhaps made using two kinds of hydrocracking catalyst gradations of two kinds of molecular sieve composite catalysts or selection
With, or inverted sequence hydrocracking process technology is used, but the product of the same fraction range of these techniques is typically only capable to production one
The product of kind specification, i.e. operating flexibility compares poor.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of flexible hydrogenation of shale oil process, i.e., by using adding
Hydrogen pretreatment technology and from using extraction section liquid phase reactor object in the middle part of the hydrocracking reactor of Y type hydrocracking catalyst
Stream, the shale oil feedstock oil is hydrocracked and heterogeneous types hydrocracking catalyst by Y type hydrocracking catalyst
Hydroisomerizing cracking combined method flexibly produce the preparing ethylene by steam cracking raw material of high quality, High Quality Lube Base Oils raw material and
The naphtha product of plurality of specifications and high-quality automotive fuel product.
Flexible hydrogenation of shale oil process of the invention, includes the following steps:
A, shale oil feedstock oil enters weighted BMO spaces reactor under the conditions of weighted BMO spaces first and passes through weighted BMO spaces
Catalyst bed, obtained weighted BMO spaces logistics in high-pressure separator isolated weighted BMO spaces high pressure hydrogen-rich gas and
Liquid phase stream；
B, the liquid phase stream that step a is obtained enters in the case where being hydrocracked pretreatment condition and is hydrocracked preatreating reactors and passes through
Pretreating catalyst by hydrocracking bed is hydrocracked pretreatment stream and passes through hydrocracking reactor under hydrocracking condition
In the first hydrocracking catalyst bed containing Y zeolite catalyst, obtain first and be hydrocracked logistics, this part reaction
Logistics is divided into two parts, and a portion is separated by gas-liquid separator, and acquired liquid stream extraction is hydrocracked anti-
Answer device；
C, in step b the first of remainder be hydrocracked logistics continuation pass through hydrocracking reactor under hydrocracking condition
In the second hydrocracking catalyst bed containing Y zeolite catalyst, be hydrocracked logistics and separated, be fractionated to obtain plus hydrogen
Cracking high pressure hydrogen-rich gas is hydrocracked gas product, hydrocracked naphtha product, is hydrocracked boat product of coal, hydrogen is added to split
Change diesel product and hydrocracking tail oil product；
D, first of extraction device obtained by step b is hydrocracked liquid phase stream under hydroisomerizing cracking conditions by adding hydrogen different
Hydroisomerizing Cracking catalyst bed in structure cracker containing heterogeneous types molecular sieve catalyst, hydroisomerizing cracking object
Flow through separation, fractionation obtains hydroisomerizing cracking high pressure hydrogen-rich gas, hydroisomerizing cracked gas product, hydroisomerizing cracking stone
Naphtha product, hydroisomerizing cracking boat product of coal, hydroisomerizing cracked diesel oil product and hydroisomerizing cracking tail oil product.
Hydrocracking process according to the present invention, wherein can also include step e: the weighted BMO spaces that step a is obtained be high
The hydroisomerizing cracking high pressure hydrogen rich gas for being hydrocracked high pressure hydrogen-rich gas and step d and obtaining that pressure hydrogen-rich gas, step c are obtained
It is recycled after body mixing.
Contain S, N, O and metal impurities in shale oil feedstock oil, especially metal will cause reactor inlet blocking to cause
Pressure drop, and pretreating catalyst by hydrocracking duct is blocked, permanent catalyst deactivation is caused, O hydrogenation reaction generates water, meeting
Cause the molecular sieve in hydrocracking catalyst to collapse, hydrocracking catalyst inactivation is caused even to crush.When feedstock oil passes through
O and metal are effectively removed when hydrogenation pretreatment catalyst, and S, N are removed to a certain extent, and aromatic hydrocarbons obtains to a certain extent
To adding hydrogen to be saturated, logistics separates water with liquid phase stream after high-pressure separator separates after weighted BMO spaces, and liquid phase stream
S, N are effectively removed when continuing through pretreating catalyst by hydrocracking, and aromatic hydrocarbons further adds hydrogen to be saturated, and are hydrocracked pre- place
It is anti-to separate ring for cyclic hydrocarbon generating unit when reason logistics continues through the hydrocracking catalyst bed containing Y zeolite catalyst
It answers, aromatic hydrocarbons further adds hydrogen to be saturated, and macromolecular is cracked into small molecule, and a part is hydrocracked logistics and continues to be hydrocracked,
Because Y type molecular sieve has the characteristics of preferential cracking macromolecular cyclic hydrocarbon, the low boat coal of available high normal hydrocarbon content, arene content
Product, diesel product and tail oil product；A part first of extraction is hydrocracked logistics by urging containing heterogeneous types molecular sieve
Continue isomery after the hydroisomerizing Cracking catalyst of agent to be hydrocracked, because heterogeneous types molecular sieve has isomery and cracking
The characteristics of, the isocraking product of available high isomery hydrocarbon content, especially gained diesel product condensation point is low, tail oil product
Condensation point it is low and viscosity index (VI) is high.
Compared with prior art, the advantages of present invention flexible hydrogenation of shale oil process, is:
1, it in the present invention, by weighted BMO spaces process, after the O in shale oil being removed and separates, avoids plus hydrogen is raw
At water detrimental effects are caused to follow-up hydrogenation Cracking catalyst and hydroisomerizing Cracking catalyst, by metal removal and remain in
Weighted BMO spaces reactor reduces the influence to preatreating reactors and catalyst is hydrocracked, and extends follow-up hydrogenation and splits
Change the service life of pretreatment catalyst, hydrocracking catalyst and hydroisomerizing Cracking catalyst.
It 2, include at least two hydrocracking catalyst beds in hydrocracking reactor in the present invention.Existed by setting
Cracking material extraction step among hydrocracking reactor bed is not necessarily to special operation, can be realized to being hydrocracked material
Effective distribution of stock, then make obtained material by different hydrocracking process, so as to flexibly produce different size
Purpose product, especially tail oil product.Meanwhile abstraction reaction logistics is technically also to be easy to real among reactor bed
Existing.And in the prior art, although by adjusting the available a variety of light-end products of boiling range of conversion ratio and adjustment product,
It is since only one hydrocracking reactor exports, a set of same fraction range of hydrocracking unit is typically only capable to one kind
Light naphtha product, heavy naphtha product, boat product of coal and the diesel product of type, especially can only obtain a kind of tail oil product；
If it is intended to obtaining the hydrocracked product of different size, two sets or more of hydrocracking unit is needed.Therefore, the present invention is for the first time
One kind is provided on a set of hydrocracking process device while producing two or more same fraction ranges, but different size tail oil
Product, two or more different sizes boat product of coal, two or more different size diesel products and a variety of different size naphthas produce
The hydrocracking process of product.
3, the present invention is hydrocracked logistics extraction by the way that first is arranged among the catalyst bed of hydrocracking reactor
Device, by shale oil raw material by weighted BMO spaces, be hydrocracked pretreatment and what is be hydrocracked first be hydrocracked liquid phase object
Stream extracts reactor, and it is anti-to be respectively fed to the hydroisomerizing cracker being separately provided progress hydroisomerizing cracking
It answers, further decreases the condensation point for being hydrocracked rear material, so that method of the invention can flexibly produce different aromatic hydrocarbons
Content, the naphtha product of different isomerization hydrocarbon content, boat product of coal, diesel product and tail oil product.
4, in the present invention, in the product that two reactor streams are fractionated, by adding hydrogen containing Y zeolite catalyst
The heavy naphtha virtue obtained after cracking is dived, and relatively high, boat product of coal smoke point is relatively high, and diesel product Cetane number is relatively
Height, tail oil product paraffinicity is high, BMCI value is relatively low；It is hydrocracked, contains containing Y zeolite catalyst by part
There are the naphtha isomery hydrocarbon content height obtained after heterogeneous types molecular sieve catalyst hydroisomerizing cracking, boat product of coal freezing point low,
Diesel product condensation point is low, and tail oil product hydrocarbon isomer content is high, viscosity index (VI) is big, condensation point is low；The different rule of production can be met respectively
The needs of the naphtha of lattice, navigate product of coal, diesel product and tail oil product.
5, in the present invention, the liquid itself obtained among hydrocracking reactor hydrocracking catalyst bed has very high
Temperature and pressure, can be directly entered in newly-installed hydroisomerizing cracker and be reacted, to make full use of
This thigh divides heat entrained by compound material, realizes that the coupling of hydroisomerizing cracker and hydrocracking reactor is grasped
Make.
Detailed description of the invention
Fig. 1 is principle process schematic diagram of the invention.
Wherein: 1- shale oil feedstock oil, 2- weighted BMO spaces reactor, 3- are hydrocracked preatreating reactors, and 4- adds hydrogen
Cracker, 5- hydroisomerizing cracked stock logistics, 6- are hydrocracked logistics, 7- hydroisomerizing cracker, and 8- adds hydrogen
Cracking high-pressure separator, 9- hydroisomerizing cracking high-pressure separator, 10- are hydrocracked fractionating column, 11- hydroisomerizing cracking fractionation
Tower, 12- are hydrocracked light naphtha product, and 13- is hydrocracked heavy naphtha product, and 14- is hydrocracked boat product of coal, and 15- adds
Hydrogen cracked diesel oil product, 16- hydrocracking tail oil product, 17- hydroisomerizing cracking light naphtha product, 18- hydroisomerizing are split
Change heavy naphtha product, 19- hydroisomerizing cracking boat product of coal, 20- hydroisomerizing cracked diesel oil product, 21- hydroisomerizing are split
Changing tail oil product, 22- is hydrocracked high-pressure separator hydrogen-rich gas, 23- hydroisomerizing cracking high-pressure separator hydrogen-rich gas,
24- supplement hydrogen, 25- weighted BMO spaces high-pressure separator, 26- weighted BMO spaces high-pressure separator hydrogen-rich gas, 27- add hydrogen to locate in advance
Manage the logistics of high-pressure separator liquid phase, 28- gas-liquid separator, 29- hydroisomerizing cracking recycle hydrogen.
Specific embodiment
The initial boiling point of shale oil raw material described in step a is 100~400 DEG C, and the end point of distillation is 400~650 DEG C.The shale
Oily feedstock oil can be the shale oil obtained in the oil shale, can also with obtained from coal coal tar, coal direct liquefaction oil,
The miscella of one or more of ICL for Indirect Coal Liquefaction oil, synthetic oil etc., can also blend the straight-run gas oil obtained from petroleum, coke
Change wax oil, catalytic cycle oil etc..
Pretreating catalyst by hydrocracking described in hydrogenation pretreatment catalyst described in step a and step b is routine
Hydrotreating catalyst.Generally using VI B race and/or group VIII metal as active component, it is with aluminium oxide or silicon-containing alumina
Carrier, group VIB metal are generally Mo and/or W, and group VIII metal is generally Co and/or Ni.With the poidometer of catalyst,
VI B race tenor is calculated as 10wt%~35wt% with oxide, and group VIII metal content is calculated as 3wt%~15wt% with oxide,
Its property is as follows: specific surface is 100~650m20.15~0.6mL/g of/g, Kong Rongwei.Main catalyst has Fushun petroleum
3936, the 3996 of work research institute development, the catalysis of the weighted BMO spaces such as FF-16, FF-26, FF-36, FF-46, FF-56 series
Agent is also possible to the function of domestic and international catalyst Co. exploitation similar to catalyst, and such as HC-K, HC-P of Uop Inc., Topsoe is public
TK-555, TK-565 catalyst and KF-847, KF-848 of Akzo company of department etc..Hydrogenation pretreatment catalyst and plus hydrogen split
Changing pretreatment catalyst can be identical, can not also be identical.Weighted BMO spaces operating condition can be used conventional operating condition, and one
As be reaction pressure 3.0MPa~19.0MPa, reaction temperature is 260 DEG C~430 DEG C, volume space velocity 0.2h when liquid-1~6.0h-1,
Hydrogen to oil volume ratio is 100:1~2000:1.
Load hydrogenation protecting agent and Hydrodemetalation catalyst in hydrogenation pretreatment catalyst top described in step a.Its
Middle hydrogenation protecting agent accounts for the 5% ~ 20% of weighted BMO spaces reactor total catalyst volume, and Hydrodemetalation catalyst accounts for plus hydrogen is located in advance
Manage the 10% ~ 40% of reactor total catalyst volume.
High-pressure separator described in step a is conventional separator, is operated under the conditions of reaction pressure.
The water or the extraneous water brought into generated in liquid phase stream described in step a without containing reaction.In liquid phase stream
Total metal contents in soil is not more than 5 μ g/g, preferably no greater than 3 μ g/g.
Pretreatment operation condition is hydrocracked described in step b can be used conventional operating condition, generally reaction pressure
3.0MPa~19.0MPa, reaction temperature are 300 DEG C~450 DEG C, volume space velocity 0.2h when liquid-1~6.0h-1, hydrogen to oil volume ratio is
100:1~2000:1.
Hydrocracking catalyst described in step b and step c is conventional hydrocracking catalyst.Generally with group VIB
And/or group VIII metal is active component, group VIB metal is generally Mo and/or W, group VIII metal be generally Co and/or
Ni.Catalyst carrier contains one of aluminium oxide, silicon-containing alumina and Y type molecular sieve or a variety of, preferably contains molecular sieve, institute
The molecular sieve stated can be Y type molecular sieve.With the poidometer of catalyst, group VIB tenor with oxide be calculated as 10wt%~
35wt%, group VIII metal content are calculated as 3wt%~15wt% with oxide, and molecular sieve content is 5wt%~80wt%.It is main to urge
Agent has the 3824 of Fushun Petrochemical Research Institute's development, 3825,3976, FC-12, FC-24, FC-26, FC-32, FC-
50 catalyst etc., HC-12, HC-14, HC-24, HC-39 etc. of Uop Inc..For hydrocracking catalyst, it is desirable that have one
Fixed hydrogenation activity and certain lytic activity should guarantee that hydrotreating generates and generate alkene in fraction in oil and hydrocracking process
Hydrocarbon and aromatic hydrocarbons plus hydrogen saturation, the aromatic hydrocarbons after also requiring saturation the reaction of open loop occurs.
Conventional operating condition can be used in the operating condition being hydrocracked described in step b, generally are as follows: reaction pressure
3.0MPa~19.0MPa, reaction temperature are 300 DEG C~450 DEG C, volume space velocity 0.2h when liquid-1~6.0h-1, hydrogen to oil volume ratio is
100:1~2000:1.
Gas-liquid separator described in step b is between hydrocracking reactor bed or what catalyst bed entrance was arranged sets
It is standby.Gas-liquid separator at least reaction stream entrance, several parts such as liquid phase conduit and gas phase conduit, wherein liquid phase conduit will separate
Obtained liquid phase pulls out hydrocracking reactor, and isolated gas phase is introduced lower part hydrocracking catalyst by gas phase conduit
Bed.
A part of first hydrocracking reaction logistics enters gas-liquid separator by gas-liquid separator entrance in step b, takes out
The weight percent that Partial Liquid Phase logistics out accounts for shale oil feedstock oil is 5~95wt%, preferably 10~80wt%.
Conventional operating condition can be used in the operating condition being hydrocracked described in step c, generally are as follows: reaction pressure
3.0MPa~19.0MPa, reaction temperature are 300 DEG C~450 DEG C, volume space velocity 0.2h when liquid-1~6.0h-1, hydrogen to oil volume ratio is
100:1~2000:1.
Separation described in step c generally comprises be hydrocracked high-pressure separator and low pressure separator separates two parts.
Its high-pressure separator is isolated to be hydrocracked high pressure hydrogen-rich gas and liquid, and the isolated liquid of high-pressure separator enters
Low pressure separator.Low pressure separator is by the isolated hydrocarbon-rich gas of highly pressurised liquid product and low pressure liquid product.Hydrocarbon-rich gas warp
Isolated needs are hydrocracked gas product.
Fractionation described in step c carries out in being hydrocracked fractionating column system.Low pressure liquid product divides in fractionating column
It evaporates to obtain and is hydrocracked light naphtha product, is hydrocracked heavy naphtha product, is hydrocracked boat product of coal, is hydrocracked diesel oil
Product and hydrocracking tail oil product.
Hydroisomerizing Cracking catalyst described in step d is conventional hydroisomerizing Cracking catalyst.Generally with group VIB
And/or group VIII metal is active component, group VIB metal is generally Mo and/or W, group VIII metal be generally Co and/or
Ni.Catalyst carrier contains one of aluminium oxide, silicon-containing alumina and molecular sieve or a variety of, preferably comprises molecular sieve, described
Molecular sieve can be for beta molecular sieve, Sapo type molecular sieve etc..With the poidometer of catalyst, group VIB tenor is to aoxidize
Object is calculated as 10wt%~35wt%, and group VIII metal content is calculated as 3wt%~15wt% with oxide, molecular sieve content be 5wt%~
80wt%.FC-14, FC-20 etc. that main catalyst has Fushun Petrochemical Research Institute to develop.It is urged for being hydrocracked
For agent, it is desirable that have certain hydrogenation activity and certain lytic activity, should guarantee alkene and aromatic hydrocarbons in reaction mass plus
Hydrogen saturation, also requires linear paraffin that isomerization reaction occurs.Conventional operating condition can be used in the operating condition of hydroisomerizing cracking,
Generally are as follows: reaction pressure 3.0MPa~19.0MPa, reaction temperature are 300 DEG C~450 DEG C, volume space velocity 0.2h when liquid-1~
6.0h-1, hydrogen to oil volume ratio is 100:1~2000:1.
Separation described in step d carries out in hydroisomerizing cracking high-pressure separator and low pressure separator.Wherein plus hydrogen
The isolated hydroisomerizing cracking high pressure hydrogen-rich gas of isocraking high-pressure separator and liquid, high-pressure separator are isolated
Liquid enters low pressure separator.Low pressure separator is by the isolated hydrocarbon-rich gas of highly pressurised liquid product and low pressure liquid product.It is rich
Appropriate hydrocarbon gas is isolated to the hydroisomerizing cracked gas product of needs.
Fractionation described in step d carries out in hydroisomerizing cracking fractionating column system.Low pressure liquid product is in fractionating column
Middle fractionation obtains hydroisomerizing cracking light naphtha product, hydroisomerizing cracking heavy naphtha product, hydroisomerizing cracking boat coal
Product, hydroisomerizing cracked diesel oil product and hydroisomerizing cracking tail oil product.
Gas product and hydroisomerizing cracked gas product are hydrocracked described in step c and step d individually to be made
For product, mixed gas product can also be mixed into.
It is hydrocracked light naphtha product described in step c and step d and hydroisomerizing cracking light naphtha product can
Mixing light naphtha product can also be mixed into separately as product.
It is hydrocracked heavy naphtha product described in step c and step d and hydroisomerizing cracking heavy naphtha product can
Mixing heavy naphtha product can also be mixed into separately as product.
Boat product of coal and hydroisomerizing cracking boat product of coal are hydrocracked described in step c and step d individually to be made
For product, mixing boat product of coal can also be mixed into.
Diesel product and hydroisomerizing cracked diesel oil product are hydrocracked described in step c and step d individually to be made
For product, mixed diesel product can also be mixed into.
Hydrocracking tail oil described in step c is separately as product.
Hydroisomerizing cracking tail oil described in step d is separately as product.
It can be used directly as recycle hydrogen after the mixing of high pressure hydrogen-rich gas described in step e, also can choose and pass through
It is recycled after desulphurization of recycle hydrogen system removing hydrogen sulfide.
In conjunction with Fig. 1, method of the invention is specific as follows: shale oil feedstock oil 1 is mixed into recycle hydrogen first plus hydrogen is pre-
Treatment reactor 2, weighted BMO spaces logistics, which enters, carries out gas-liquid separation in weighted BMO spaces high-pressure separator 25, isolated to add
Hydrogen pretreatment high-pressure separator high pressure hydrogen-rich gas 26 and weighted BMO spaces high-pressure separator liquid phase logistics 27, liquid phase stream 27 with
Recycle hydrogen, which is mixed into, is hydrocracked preatreating reactors 3, is hydrocracked pretreatment stream continuation and recycle hydrogen is mixed into and adds
Hydrogen cracker 4 enters in gas-liquid separator 28 by a part in the reaction stream of the first hydrocracking catalyst bed,
Isolated liquid phase extraction is used as hydroisomerizing cracked stock logistics 5, the logistics after extracting hydroisomerizing cracked stock logistics 5 out
Follow-up hydrogenation Cracking catalyst bed is gone successively to, is hydrocracked to generate logistics 6 and enter and is hydrocracked high-pressure separator 8 and carries out gas
Liquid separation, isolated liquid enter fractionation in fractionating column 10 and obtain being hydrocracked light naphtha product 12, are hydrocracked weight
Naphtha product 14 is hydrocracked boat product of coal 14, is hydrocracked diesel product 15 and hydrocracking tail oil product 16, adds hydrogen different
Structure cracked stock logistics 5 enters hydroisomerizing cracker 7 after mixing with hydroisomerizing cracking recycle hydrogen 29, by adding hydrogen different
The product stream of structure Cracking catalyst bed, which enters in hydroisomerizing cracking high-pressure separator 9, carries out gas-liquid separation, isolated
Liquid enter in fractionating column 11 that fractionation obtains hydroisomerizing cracking light naphtha product 17, hydroisomerizing cracking heavy naphtha produces
Product 18, hydroisomerizing cracking boat product of coal 19, hydroisomerizing cracked diesel oil product 20 and hydroisomerizing cracking tail oil product 21, add
Hydrogen cracking light naphtha product 12 and hydroisomerizing cracking light naphtha product 17 can be separately as products, after can also mixing
Mixing light naphtha product is obtained, heavy naphtha product 13 is hydrocracked and hydroisomerizing cracking heavy naphtha product 18 can be single
It is solely used as product, mixing heavy naphtha product is obtained after can also mixing, is hydrocracked boat product of coal 14 and hydroisomerizing cracking
The product of coal 19 that navigates can obtain mixing boat product of coal, be hydrocracked 15 He of diesel product separately as product after can also mixing
Hydroisomerizing cracked diesel oil product 20 can obtain mixed diesel product, be hydrocracked separately as product after can also mixing
Isolated 23 and of hydrogen-rich gas of the isolated hydrogen-rich gas 22 of high-pressure separator 8, hydroisomerizing cracking high-pressure separator 9
The isolated hydrogen-rich gas 26 of weighted BMO spaces high-pressure separator 25 mix after after circulating hydrogen compressor is pressurized with supplement hydrogen
24 mixing are used as recycle hydrogen.
Illustrate the present invention program and effect below by embodiment.
Embodiment 1-3
Protective agent FZC-100, FZC-105 and FZC106 are China Petroleum and Chemical Corporation Fushun Petrochemical Research Institute
The hydrogenation protecting agent of development and production；Catalyst FZC-204 is the petrochemical industry research of Sinopec Group Fushun
The Hydrodemetalation catalyst of institute's development and production；Catalyst FF-56 is Sinopec Group Fushun petroleum
The hydrotreating catalyst of work research institute development and production；Catalyst FC-32 is Sinopec Group Fushun stone
The catalyst for hydro-upgrading of oily chemical research institute's development and production, contains Y type molecular sieve；Catalyst FC-20 is Sinopec
The hydroisomerizing Cracking catalyst of Fushun Petrochemical Research Institute, limited liability company development and production, contains beta molecular sieve.
The main character of 1 shale oil feedstock oil of table
2 process conditions of table
2 process conditions of continued
3 test result of table
Using flexible hydrogenation of shale oil process of the invention it can be seen from embodiment, by using weighted BMO spaces and
Product flow separation is pre-processed, and extracts a part of reaction stream out out of hydrocracking reactor, and uses hydrocracking catalyst
Agent and hydroisomerizing Cracking catalyst are flexible to realize the purpose of production heterogeneity hydrocracked product, production method.
Claims (16)
1. a kind of flexible hydrogenation of shale oil process, includes the following steps:
A, shale oil feedstock oil enters weighted BMO spaces reactor under the conditions of weighted BMO spaces first and passes through weighted BMO spaces
Catalyst bed, obtained weighted BMO spaces logistics in high-pressure separator isolated weighted BMO spaces high pressure hydrogen-rich gas and
Liquid phase stream；
B, the liquid phase stream that step a is obtained enters in the case where being hydrocracked pretreatment condition and is hydrocracked preatreating reactors and passes through
Pretreating catalyst by hydrocracking bed is hydrocracked pretreatment stream and passes through hydrocracking reactor under hydrocracking condition
In the first hydrocracking catalyst bed containing Y zeolite catalyst, obtain first and be hydrocracked logistics, this part reaction
Logistics is divided into two parts, and a portion is separated by gas-liquid separator, and acquired liquid stream extraction is hydrocracked anti-
Answer device；
C, in step b the first of remainder be hydrocracked logistics continuation pass through hydrocracking reactor under hydrocracking condition
In the second hydrocracking catalyst bed containing Y zeolite catalyst, be hydrocracked logistics and separated, be fractionated to obtain plus hydrogen
Cracking high pressure hydrogen-rich gas is hydrocracked gas product, hydrocracked naphtha product, is hydrocracked boat product of coal, hydrogen is added to split
Change diesel product and hydrocracking tail oil product；
D, first of extraction device obtained by step b is hydrocracked liquid phase stream under hydroisomerizing cracking conditions by adding hydrogen different
Hydroisomerizing Cracking catalyst bed in structure cracker containing heterogeneous types molecular sieve catalyst, hydroisomerizing cracking object
Flow through separation, fractionation obtains hydroisomerizing cracking high pressure hydrogen-rich gas, hydroisomerizing cracked gas product, hydroisomerizing cracking stone
Naphtha product, hydroisomerizing cracking boat product of coal, hydroisomerizing cracked diesel oil product and hydroisomerizing cracking tail oil product.
2. hydrocracking process described in accordance with the claim 1, which is characterized in that further include step e: step a is obtained plus hydrogen
It is high that pretreatment high pressure hydrogen-rich gas, step c were obtained is hydrocracked the hydroisomerizing cracking that high pressure hydrogen-rich gas and step d are obtained
It is recycled after pressure hydrogen-rich gas mixing.
3. hydrocracking process described in accordance with the claim 1, which is characterized in that the initial boiling point of shale oil raw material described in step a
It is 100~400 DEG C, the end point of distillation is 405~650 DEG C.
4. hydrocracking process according to claim 2, which is characterized in that also blend coal in the shale oil feedstock oil
One of tar, coal direct liquefaction oil, ICL for Indirect Coal Liquefaction oil, synthetic oil, straight-run gas oil, wax tailings, catalytic cycle oil or
It is several.
5. hydrocracking process described in accordance with the claim 1, which is characterized in that hydrogenation pretreatment catalyst described in step a
With pretreating catalyst by hydrocracking described in step b using VI B race and/or group VIII metal as active component, with aluminium oxide
Or silicon-containing alumina is carrier；With the poidometer of catalyst, group VIB tenor is calculated as 10wt%~35wt% with oxide,
Group VIII metal content is calculated as 3wt%~15wt% with oxide；Its property is as follows: specific surface area is 100~650m2/ g, Kong Rong
For 0.15~0.6mL/g.
6. hydrocracking process described in accordance with the claim 1, which is characterized in that weighted BMO spaces condition described in step a are as follows:
Reaction pressure 3.0MPa~19.0MPa, reaction temperature are 260 DEG C~430 DEG C, volume space velocity 0.2h when liquid-1~6.0h-1, hydrogen oil
Volume ratio is 100:1~2000:1.
7. hydrocracking process described in accordance with the claim 1, which is characterized in that the catalysis of weighted BMO spaces described in step a
Filling hydrogenation protecting agent and Hydrodemetalation catalyst above agent；Hydrogenation protecting agent accounts for weighted BMO spaces reactor total catalyst body
Long-pending 5% ~ 20%, Hydrodemetalation catalyst account for the 10% ~ 40% of weighted BMO spaces reactor total catalyst volume.
8. hydrocracking process described in accordance with the claim 1, which is characterized in that be free of in liquid phase stream described in step a
There is reaction to generate water or the extraneous water brought into.
9. hydrocracking process described in accordance with the claim 1, which is characterized in that total metal in the liquid phase stream that step a is obtained
Content is not more than 5 μ g/g, preferably no greater than 3 μ g/g.
10. hydrocracking process described in accordance with the claim 1, which is characterized in that be hydrocracked pretreatment item described in step b
Part are as follows: reaction pressure 3.0MPa~19.0MPa, reaction temperature are 300 DEG C~450 DEG C, volume space velocity 0.2h when liquid-1~6.0h-1, hydrogen to oil volume ratio is 100:1~2000:1.
11. hydrocracking process described in accordance with the claim 1, which is characterized in that be hydrocracked described in step b and step c
Catalyst is using group VIB and/or group VIII metal as active component, and catalyst carrier contains aluminium oxide and/or siliceous oxidation
Aluminium and Y type molecular sieve；With the poidometer of catalyst, group VIB tenor is calculated as 10wt%~35wt%, the VIIIth race with oxide
Tenor is calculated as 3wt%~15wt% with oxide, and Y type molecular sieve content is 5wt%~80wt%.
12. hydrocracking process described in accordance with the claim 1, which is characterized in that the hydrocracking condition in step b
Are as follows: reaction pressure 3.0MPa~19.0MPa, reaction temperature are 300 DEG C~450 DEG C, volume space velocity 0.2h when liquid-1~6.0h-1,
Hydrogen to oil volume ratio is 100:1~2000:1.
13. hydrocracking process described in accordance with the claim 1, which is characterized in that the liquid phase stream extracted out in step b accounts for raw material
The weight percent of oil is 5~95 wt%, preferably 10~80 wt%.
14. hydrocracking process described in accordance with the claim 1, which is characterized in that hydrocracking condition described in step c
Are as follows: reaction pressure 3.0MPa~19.0MPa, reaction temperature are 300 DEG C~450 DEG C, volume space velocity 0.2h when liquid-1~6.0h-1,
Hydrogen to oil volume ratio is 100:1~2000:1.
15. hydrocracking process described in accordance with the claim 1, which is characterized in that hydroisomerizing cracking catalysis described in step d
Agent using group VIB and/or group VIII metal as active component, the carrier of catalyst contain aluminium oxide and/or silicon-containing alumina and
Molecular sieve, the molecular sieve are beta molecular sieve or Sapo type molecular sieve；With the poidometer of catalyst, group VIB tenor
It is calculated as 10wt%~35wt% with oxide, group VIII metal content is calculated as 3wt%~15wt% with oxide, and molecular sieve content is
5wt%~80wt%.
16. hydrocracking process described in accordance with the claim 1, which is characterized in that the hydroisomerizing cracking conditions are as follows: anti-
Answer pressure 3.0MPa~19.0MPa, reaction temperature is 300 DEG C~450 DEG C, volume space velocity 0.2h when liquid-1~6.0h-1, hydrogen oil body
Product is than being 100:1~2000:1.
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| CN114437804A (en) * | 2020-10-19 | 2022-05-06 | 中国石油化工股份有限公司 | Hydrocracking method of high-nitrogen raw oil |
| CN114437798A (en) * | 2020-10-19 | 2022-05-06 | 中国石油化工股份有限公司 | Shale oil hydrocracking method |
| CN114437799A (en) * | 2020-10-19 | 2022-05-06 | 中国石油化工股份有限公司 | Hydrocracking method |
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| CN114437804A (en) * | 2020-10-19 | 2022-05-06 | 中国石油化工股份有限公司 | Hydrocracking method of high-nitrogen raw oil |
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| CN114437799A (en) * | 2020-10-19 | 2022-05-06 | 中国石油化工股份有限公司 | Hydrocracking method |
| CN114437798B (en) * | 2020-10-19 | 2023-05-30 | 中国石油化工股份有限公司 | Shale oil hydrocracking method |
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