CN106147835B - A kind of separation catalytic cracked oil pulp simultaneously prepares the combined method that oil is needle coke - Google Patents
A kind of separation catalytic cracked oil pulp simultaneously prepares the combined method that oil is needle coke Download PDFInfo
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Abstract
The present invention provides a kind of separation catalytic cracked oil pulp and prepares the combined method that oil is needle coke.Extractant is made using C3 C5 light ends fractionations, subcritical or supercritical extract is carried out to catalytic cracked oil pulp, extracted component is made through supercritical recovery solvent to obtained extraction oil phase, raw material is prepared using extracted component as mesophase pitch, mesophase pitch is prepared through thermal polycondensation reaction, then the delayed pyrogenetic reaction of mesophase pitch is prepared to the oil system needle coke of high-quality.When the sulfur content of catalytic cracked oil pulp is higher, light component first hydrogenated desulfurization process can will be extracted, carrying out fractionation to hydrogenated oil collects hydrogenation tail oil, prepares raw material using hydrogenation tail oil as mesophase pitch, and then prepare needle coke.The method of the present invention is mutual indepedent by the preparation of control mesophase pitch and the coking process of needle coke, more conducively realization of industrialization, and can make full use of catalytic cracked oil pulp and prepare the needle coke material of high-quality.
Description
Technical field
The combined method that oil is needle coke is detached and prepared the present invention relates to catalytic cracked oil pulp, specifically includes separation catalysis
Cracking slurry oil and delayed coking production oil are the group technology of needle coke.
Background technology
Needle coke is a kind of carbon material, is mainly used for the production of high power and ultra high power graphite electrode.According to preparation
The difference of raw material sources, needle coke be divided into oil system and two class of coal measures, wherein oil system needle coke be by oil plant processing of heavy oil and
At application is more extensive, and market demand is very big, but production capacity is insufficient.In the prior art, production oil system needle coke
Delay coking process, including three feedstock oil pretreatment, delayed coking green coke and calcining parts are generally used, but in actual industrial
There are feed purification and coking technology controlling and process this two big technological difficulties in production, thus the needle coke product pair of high-quality to be obtained
Technology controlling and process proposes higher requirement.Using feedstock oil produce needle coke process include：Feedstock oil is preprocessed, reacts
Mesophase pitch is first prepared, then needle coke is generated using the delayed coking of the mesophase pitch, calcining, so, interphase
Pitch is not only the important intermediate raw material of production needle coke, and the quality of mesophase pitch can also influence the quality of needle coke.
With the popularization and application of Catalytic Cracking Technique of Heavy Oil, the quantity of catalytic cracking unit byproduct slurry oil (FCC slurry)
Increasing, China's catalytic cracking unit working ability reaches 200,000,000 tons, and conservative estimation whole nation slurry oil yield is about at 7,500,000 tons/year
More than.The processing and utilization of slurry oil are also increasingly concerned in processing of heavy oil field, and current present situation is most of cycle oil
Slurry mixes fuel oil or directly as fuel oil, and also for part slurry oil as pitch blend component, this does not make good use of treasured not only
Expensive petroleum resources, and in combustion due to the presence of the impurity such as residual catalyst easily cause heating furnace fire nozzle abrasion and
Coking.The refineries Ye You reduce to the greatest extent and are got rid of outside slurry oil for economic benefit considers, but the cracking reaction performance of catalytic cracked oil pulp
Difference, conversion ratio and light oil yield are all very low, are allowed to constantly accumulate the coking for recycling and leading to catalyst in catalytic cracking unit
Inactivation aggravation, to make catalyst consumption increase, things turn out contrary to one's wishes for final result, and economic benefit is deteriorated instead.
There is the component rich in aromatic hydrocarbons in FCC slurry, is that valuable industrial chemicals and carbon material prepare raw material, can be used for producing
Various aromatic naphtha and raw material as mesophase pitch, so and production needle coke raw material.But catalytic slurry is very multiple
Miscellaneous system, colloid, asphalitine and a small amount of other solid impurities therein, if cannot be effectively treated and directly produce
Mesophase pitch can lead to mosaic texture, it is difficult to form high-quality mesophase pitch, more affect the quality of needle coke.
So how effectively refining catalytic cracking slurry oil raw material just become make good use of slurry oil raw material prepare high-quality among
Asphalt phase and then one of the critical issue for obtaining high quality oils system needle coke.For the solid impurity in slurry oil, the methods of filtering
It is only capable of detaching wherein larger particulate matter, solid particle compared with small particle, such as catalyst fines etc. is then difficult to detach, less
The components such as asphalitine therein can be removed.Vacuum distillation and solvent extraction are common Heavy oil separation methods, but are evaporated under reduced pressure and dial
Extracting rate is limited, if wanting, the dial-out rate for improving distillation is bound to vapo(u)rizing temperature to be improved, and since slurry oil condensed-nuclei aromatics content is high, and also has
The impurity such as asphalitine, high temperature distillation easily cause heating furnace and destilling tower coking, are not only difficult to improve the extracting rate of extract, also make
Shortened equipment life.As for using solvent extraction technology, the operation for having research and being known together is tried aromatic component from slurry oil
Separate that be pursued target can extract the solvent of aromatic hydrocarbons to take out so according to the property of catalytic cracked oil pulp using furfural etc.
It is studied at present and concern technique direction to propose separation, but problems faced is to this kind of body of slurry oil in industrialized production
System, since gum asphalt also is extracted out simultaneously, is not only difficult to realize extraction although furfural class solvent can extract aromatic hydrocarbons
Object is taken to be detached with the split-phase of non-aromatics, it is also difficult to reach the refined purpose of slurry oil raw material, it is therefore desirable to carry out depitching to slurry oil
The pretreatment of matter and solid impurity could apply such technology.In another aspect, the property and catalytic cracking process of crude oil also cause
The difference of slurry oil property can seriously affect mesophase pitch especially for the slurry oil of high-sulfur aromatic component directly as raw material
With the quality of needle coke, but slurry oil direct hydrogenation is handled, and the impurity in slurry oil can cause catalyst bed to block and catalysis quickly
Agent is failed, just more undesirable in industrialized production, and inherently mesophase pitch produces the problem faced, this is just subsequently adopted
With mesophase pitch preparation high-quality needle coke product, this technique brings technical barrier.
In addition, the technique for preparing needle coke at present is essentially all using delayed coking unit, coking plant should be completed
The synthesis of mesophase pitch completes pyrogenetic reaction and prepares needle coke again, it is therefore desirable to change process conditions in each cycle,
Temperature and pressure variation is all bigger, causes coking technology controlling and process difficult, it is difficult to ensure the quality of needle coke.
Invention content
The present invention proposes a kind of combined method detached to catalytic cracked oil pulp and prepare that oil is needle coke, is split using catalysis
Carburetion slurry is used as raw material, the method for the more reasonable science of use to carry out separating treatment, and and mesophase pitch to catalytic cracked oil pulp
Preparation process and delay coking process it is combined, but prepare and the thermal polycondensation process of mesophase pitch and prepare the coke of needle coke
The control of chemical industry sequence is mutual indepedent, more conducively realization of industrialization, and can make full use of catalytic cracked oil pulp and prepare high-quality
Needle coke material.
The present invention provides a kind of to detach catalytic cracked oil pulp and preparing the combined method that oil is needle coke, including as follows
Step：
Make catalytic cracked oil pulp raw material and extractant counter current contacting in extraction tower, and the extractant is made to face super
The extraction to catalytic cracked oil pulp is realized under boundary or undercritical conditions, forms extraction oil phase and raffinate phase, and extraction oil phase is carried out
Overcritical separating and extracting solvent, obtains extracted component, and raffinate phase then obtains raffinate heavy constituent after recovered extractant；
Raw material is prepared using the extracted component as mesophase pitch, thermal polycondensation reaction is carried out and mesophase pitch is made；
Using obtained mesophase pitch, oil system needle coke is prepared using Delayed Coking Technology；
Wherein,
The group of the extractant is divided into C3-C5 light ends fractionations, and its pseudocritical temperature Tc is at 90 DEG C -196 DEG C, the vacation
Critical temperature Tc presses formulaIt obtains, x in formulaiIt is the molar fraction of the component i in the light ends fractionation, TciIt is the group
Divide the critical-temperature of i, n is the number of components contained by the extractant.
Combined method according to the present invention, using catalytic cracked oil pulp be raw material, include mesophase pitch preparation and
Further coking prepares the process of needle coke.To in the processing of catalytic cracked oil pulp, being used as and extracting first with selected lighter hydrocarbons
It takes solvent, control to be extracted to catalytic cracked oil pulp under the subcritical or super critical condition of the extractant, removes slurry oil
It is also removed while middle impurity and harmful asphalitine and part colloid is generated to mesophase pitch, catalytic cracked oil pulp carried out pure
While change, obtained extraction oil phase also achieves the concentration of aromatic component, coordinates the overcritical separating technology to extracting oil phase,
Prepare the mesophase pitch of high-quality to obtain the raw material of quality improving for thermal polycondensation, then by by mesophase pitch delay coke
Change prepares needle coke, realizes thermal polycondensation process and is decoupled with delayed coking process, it is anti-with coking to solve mesophase pitch synthesis
The contradiction in condition is answered, and then high quality oils system needle coke product is prepared.
Combined method according to the present invention carries out overcritical separating and extracting solvent to extraction oil phase, obtains extracted component, select
The extracted component is selected as raw material, implements pyrocondensation polymerizing technology, conducive to the mesophase pitch of high-quality is obtained, in conjunction with delayed coking
Technology obtains oil system needle coke product.
In further embodiment, mesophase pitch is prepared into raw material progress thermal polycondensation reaction, mesophase pitch is made
When, reaction pressure 0.1-3.0MPa, 400-490 DEG C of reaction temperature, reaction time 3-12h.
In further embodiment, when needle coke is made in the delayed pyrogenetic reaction of mesophase pitch, raw material is into tower temperature
480-510 DEG C of degree, reaction pressure 0.1-1.0MPa, reaction time 12-36h.Delayed coking is implemented to mesophase pitch and prepares needle
The concrete operations of shape coke can be identical with the prior art, and the present invention is not particularly limited.Such as production in can be two coke
Tower or three coke drum handover operations, during pyrogenetic reaction, reaction oil gas is flowed out from coke drum top, and the needle coke of generation stays
In coke drum, in the coke drum decoking for completing green coke, other coke drum implements reaction for continuing, for from coke drum
Obtained needle coke, through further high-temperature calcination (general 1300-1500 DEG C) to get the oil system needle coke product of high-quality.
The difference of oil property and processing technology results in the composition for being formed by catalytic cracked oil pulp and property obviously not
Together, especially high sulfur content slurry oil, following process could be used for by needing first to remove sulphur content, but is directly implemented desulfurization and easily caused to urge
Change the failure of bed.So the embodiment that the present invention detaches catalytic cracked oil pulp can also include hydrodesulfurization process, that is, if
Sulfur content >=0.5m% of the catalytic cracked oil pulp raw material, the combined method further include：
By the first hydrogenated desulfurization process of the extracted component, treated hydrogenated oil carries out fractionation collects plus hydrogen light fraction and
Hydrogenation tail oil, fraction cut point is 350-450 DEG C, and boiling point is higher than sulfur content≤0.3m% of the hydrogenation tail oil of cut point, close
Degree is in 0.970g/cm3-1.050g/cm3, arene content is in 40-65m%；
The hydrogenation tail oil prepares raw material as mesophase pitch.
In specific embodiment provided by the invention, for sulfur content >=0.5m% situations of catalytic cracked oil pulp raw material,
When first implementing hydrodesulfurization processing to the extracted component, residuum hydrodesulfurization catalyst, hydroprocessing pressure 6- may be used
16MPa, hydrogen to oil volume ratio 200:1-1200:1, air speed 0.2-2.0h-1。
For high sulphur content slurry oil, the present invention program is to implement hydrodesulfurization again after formerly removing raffinate heavy constituent, is also solved
The problem of hydrotreated feedstock is used as in the case of aromatic component high-sulfur, and the product after high-sulfur aromatic component hydrodesulfurization is made
Raw material is prepared for mesophase pitch, obtained high-quality mesophase pitch raw material is prepared high-quality interphase through thermal polycondensation and drips
Blueness is more advantageous to high quality oils system needle coke product is prepared in this way.
For catalytic cracked oil pulp in most cases, combined method of the invention may include first being carried out to extraction system
The process of separation, that is,
Make catalytic cracked oil pulp raw material and extractant counter current contacting in extraction tower, and the extractant is made to face super
Catalytic cracked oil pulp is extracted under boundary or undercritical conditions, forms extraction oil phase and raffinate phase, extraction oil phase is sent into and is divided
It is separated into light oil phase and heavy oil phase from heating in tower, and raffinate phase then obtains raffinate heavy constituent after recovered extractant；
Overcritical separating and extracting solvent is mutually carried out to the light oil, obtains extraction light component, and the heavy oil is mutually molten through detaching
Extraction intermediate species is obtained after agent；
Using the extraction intermediate species or the extraction intermediate species and the mixture of the extraction light component as centre
Asphalt phase prepares raw material, carries out thermal polycondensation reaction and mesophase pitch is made, the quality of the extraction light component in the mixture contains
Amount is no more than 50%；
Using obtained mesophase pitch, oil system needle coke is prepared using Delayed Coking Technology.
So provided by the invention includes catalytic cracked oil pulp being detached and being prepared the combined method that oil is needle coke, packet
It has included lighter hydrocarbons solvent and has extracted the necessary heavy and light oil of catalytic cracked oil pulp raw material, extraction system under overcritical or subcritical state
Mesophase pitch is prepared from processing and overcritical separation solvent, necessary hydrodesulfurization processing, thermal polycondensation and prepared by delayed coking
Needle coke process becomes the group technology being mutually matched, and can not only realize the refined of slurry oil, make full use of catalytic cracked oil pulp,
And utilize obtained polycondensation of raw materials that high-quality mesophase pitch product (its wide area anisotropic structure ratio is prepared
Can be obviously improved, 90% or more can be reached), while by decoupling the preparation of mesophase pitch and coking process, more conducively
Realization of industrialization also solves mesophase pitch synthesis and the contradiction in pyrogenetic reaction condition, further solves coking technique
Difficult problem is controlled, and then obtains high-quality needle coke.
Description of the drawings
Fig. 1 is the combined method embodiment provided by the invention detached to catalytic cracked oil pulp and prepare that oil is needle coke
Process flow diagram.
Specific implementation mode
The present invention provides it is a kind of include that extraction and separation are carried out to catalytic cracked oil pulp and prepare the combined method of needle coke,
Use the light ends fractionation of C3-C5 as extractant first as aforementioned, under the subcritical or super critical condition of the extractant
Catalytic cracked oil pulp extract and obtains extracted component through detaching or recycling extractant, the major impurity ash content in slurry oil
It is removed to raffinate heavy constituent with catalyst granules etc., while also by almost all C7 asphalitines (N.heptane insolubles) and part
Weight colloid is separated to raffinate heavy constituent, and the concentration of aromatic component in slurry oil is realized by the removing of bad component；And overcritical point
The extracted component obtained from extractant then can be used as the raw material for preparing mesophase pitch；It is former to the slurry oil of sulfur content >=0.5m%
Material, further combined with hydrodesulfurization, makes the sulfur content that intermediate pitch mutually prepares raw material be lowered, and other impurity contents,
C7 asphalitines and total metal content also further decrease, and the quality of gained needle coke product is also further promoted.
Further scheme can be first to extracting oil phase for the catalytic cracked oil pulp raw material that most of techniques obtain
It is detached, and then mesophase pitch is made and prepares raw material, will have broader adaptability, especially for not being very heavy
Slurry oil, separation catalytic cracked oil pulp of the invention simultaneously prepare the combined method that oil is needle coke, may include steps of：
Make catalytic cracked oil pulp raw material and extractant counter current contacting in extraction tower, and the extractant is made to face super
Catalytic cracked oil pulp is extracted under boundary or undercritical conditions, forms extraction oil phase and raffinate phase, extraction oil phase is sent into and is divided
It is separated into light oil phase and heavy oil phase from heating in tower, and raffinate phase then obtains raffinate heavy constituent after recovered extractant；
Overcritical separating and extracting solvent is mutually carried out to the light oil, obtains extraction light component, and the heavy oil is mutually molten through detaching
Extraction intermediate species is obtained after agent；
Using the extraction intermediate species or the extraction intermediate species and the mixture of the extraction light component as centre
Asphalt phase prepares raw material, carries out thermal polycondensation reaction and mesophase pitch is made, the quality of the extraction light component in the mixture contains
Amount is no more than 50%；
Using obtained mesophase pitch, oil system needle coke is prepared using Delayed Coking Technology；
Wherein,
The group of the extractant is divided into C3-C5 light ends fractionations, and its pseudocritical temperature Tc is at 90 DEG C -196 DEG C, the vacation
Critical temperature Tc presses formulaIt obtains, x in formulaiIt is the molar fraction of the component i in the light ends fractionation, TciIt is the group
Divide the critical-temperature of i, n is the number of components contained by the extractant.
In specific embodiments of the present invention, supercritical extract is carried out to slurry oil using lighter hydrocarbons solvent, routine can be selected
Extraction tower makes catalytic cracked oil pulp raw material as long as realizing solvent and slurry oil counter current contacting, such as sieve-plate tower or packed tower
From extraction tower top into tower and inlet temperature of stabilizer is at 70-200 DEG C, and extractant is from tower bottom into tower and inlet temperature of stabilizer is at 50 DEG C -180
DEG C, extraction pressure tower is 3.0-10.0MPa, mass ratio (agent oil quality ratio) 1.5- of extractant and catalytic cracked oil pulp raw material
5.0:1, the extraction oil phase is isolated from tower top, the raffinate phase is isolated from bottom of tower.
Based on the research of property and composition to catalytic cracked oil pulp, the present invention has selected C3-C5 lighter hydrocarbons solvent first to oil
Slurry is extracted (control subcritical or super critical condition), using such extractant and corresponding extraction conditions to slurry oil into
Row component extracts, and further the extraction light component after separation and extraction intermediate species are substantially free of asphalitine and solid (ash content),
Not only later separation intractability reduces, but also obtained thermal polycondensation raw material is conducive to prepare the mesophase pitch of quality-improving, example
If wide area anisotropic structure ratio improves, the mesophase pitch of high-quality is more conducive to obtain the needle coke product of high-quality.
Present invention lighter hydrocarbons solvent selected to use is that group is divided into C3-C5 light hydrocarbon mixtures, generally can be positive structure/isomeric alkane
Hydrocarbon and alkene, for example, can include propane, propylene, iso-butane, normal butane, butene-1, butene-2, isobutene, pentane, different
Component some or all of in pentane, neopentane and C5 alkene.Appropriate carbon number can be selected according to the property of slurry oil and composition
The hydrocarbon component, " weight " and " light " of solvent is determined in other words, for example, slurry oil density height, then select " to lay particular stress on " (carbon number is slightly higher)
Solvent composition.And the concrete scheme detached to extraction oil phase can be that extraction oil heat phase is warming up to higher than extraction tower
It pushes up 5-90 DEG C of temperature and enters knockout tower, control separating pressure is 3.0-10.0MPa, and the knockout tower can be selected from void tower, sieve-plate tower
Or packed tower, the heavy oil are mutually discharged from bottom of tower, the extraction intermediate species are obtained after detaching solvent, the light oil is mutually from tower
Top separates, and extractant is isolated through overcritical, obtains the extraction light component.The present invention uses the lighter hydrocarbons solvent, full
The required effect of extracting of foot simultaneously, is also conducive to solvent being isolated from extraction oil phase intermediate to can be used for thermal polycondensation preparation
The raw material of asphalt phase, that is, while meeting the split-phase and separating effect of the extraction to slurry oil component and extraction system.It is also based on
The lighter hydrocarbons solvent of selection C3-C5 of the invention goes out to extract intermediate species simultaneously for extraction separation of oil, and the light oil separated is mutually
Supercritical process recycling design may be used.Corresponding super critical condition is controlled according to used lighter hydrocarbons solvent property, by true
Determine separating pressure appropriate and solvent is enable mutually to be recovered with single fluid, realizes the separation with extraction slurry oil.Overcritical
Under state and the separating pressure of setting, theoretically separation temperature is higher, and the density of solvent is lower, and fluid velocity is also faster, is
Carrying of the solvent to light oil phase is reduced, also corresponding higher is required for operating cost and control.The present invention is in specific embodiment
In, when through overcritical separating and extracting solvent, the density of solvent is made to be less than 0.20g/cm3, separating pressure 3.0-10.0MPa, and
Separation temperature control is not higher than 280 DEG C.
Catalytic cracked oil pulp of the present invention from oil refining processing catalytic cracking process by-product, oil property and
Processing technology difference can also be such that slurry oil by-product be discharged has differences, can generally be reflected in sulfur content, asphalt content with
And in the indexs such as granule foreign content, the present invention does not specially require it, but consider from operation and control and product qualities, for
The slurry oil raw material of quality excessively pessimum also can in advance be handled by appropriate means.What is be applicable in specific embodiments of the present invention urges
Change cracking slurry oil raw material, generally can be：Density 0.970g/cm3-1.200g/cm3, and slurry oil carbon residue<21.0m%, C7 are dripped
Green matter content<10.0m%, ash content<3.0m%, sulfur content<3.0m%.Further selection is, for relatively " weight "
Slurry oil raw material, such as density 1.000g/cm3-1.200g/cm3, the extraction oil phase after extraction can also be detached without knockout tower
It handles and is directly transferred to supercritical recovery solvent process.
Sulfur content is to evaluate an important indicator of slurry oil property, and excessive sulphur, which brings thermal polycondensation raw material into, certainly will influence polycondensation production
The quality of object.Although it is a kind of feasible scheme first to implement desulfurization using means appropriate to slurry oil raw material before extraction and separation,
But it is damage and the catalyst failure to catalyst bed that slurry oil direct hydrogenation desulfurization, which needs the problem solved, and industry is caused to be answered
With being obstructed, so, for the higher slurry oil of sulfur content in embodiment of the present invention, first through lighter hydrocarbons solvent extraction and separation, by institute
The extraction intermediate species collected extracts intermediate species and extracts the first hydrogenated desulfurization process of mixture of light component, in slurry oil
Asphalitine and the ingredients such as colloid be removed, be used as hydrodesulfurization raw material at this time, either charging or detach and can be easy to grasp
Control.The specific processing of hydrodesulfurization can then select conventional method, include use and the treatment process determination of catalyst.
In specific embodiment provided by the invention, for the sulfur content of catalytic cracked oil pulp raw material<0.5m% slurry oils, will
Isolated extraction intermediate species, raw material is prepared directly as mesophase pitch, alternatively, with obtained extraction light component by one
Certainty ratio mixing prepares raw material (mixed raw material) as mesophase pitch, and mesophase pitch is prepared through thermal polycondensation.Mixed proportion can
To be expressed as：Extract light component:Extract intermediate species=0%-50%:100%-50%, the specific determination of mixed proportion can be with
According to the original yield ratio of separation product, for example, the density of control mixed raw material is in 1.0-1.1g/cm3, sulfur content≤
0.4m%, arene content 40m%-65m% can also adjust the heat for using while arene content in ensuring thermal polycondensation raw material
Polycondensation of raw materials amount improves the yield of mesophase pitch, certainly, after extraction and separation are handled, obtained mixed raw material impurity level
It is then obviously controlled, that is, content of ashes<0.01%, C7 asphalitine<0.1%, W metal, the total content of V, Al, Fe, Na and Ca<
5μg/g.The processing of thermal polycondensation raw material is also conducive to make prepared mesophase pitch wide area anisotropic structure ratio height (90%
More than), to provide the quality raw materials for preparing high-quality needle coke.
In specific embodiment provided by the invention, for sulfur content >=0.5m% situations of catalytic cracked oil pulp raw material,
To the extraction intermediate species or extracts intermediate species and first implement hydrodesulfurization processing with the mixture for extracting light component, it can be with
Using residuum hydrodesulfurization catalyst, hydroprocessing pressure 6-16MPa, hydrogen to oil volume ratio 200:1-1200:1, air speed 0.2-
2.0h-1。
In said program, mild hydrogenation desulfurization is implemented for extraction fraction and is advantageous, is avoided as possible in hydrodesulfurization
Overcracking, therefore the desulphurization catalyst of residual hydrocracking can be selected, conducive to the hydrogenation technique mitigated as far as possible is used,
I.e. temperature is as low as possible, and coordinates pressure, hydrogen-oil ratio and air speed appropriate.The residuum hydrodesulfurization catalyst, is heavy oil
The common and well known a kind of hydrogenation catalyst of manufacture field, is a kind of γ-Al2O3Load VIII race and/or VI B races metallic element (example
As loaded Co and Mo or Ni and W) it is active component, there are certain Kong Rong and the catalyst of pore size distribution, the present invention not special
It limits, is all from commercially available.
Treated, and system, that is, hydrogenated oil carries out that fractionation collects plus hydrogen light fraction and hydrogenation tail oil, and fraction cut point is located at
350-450 DEG C, and boiling point, higher than sulfur content≤0.3m% of the hydrogenation tail oil of cut point, density is in 0.970g/cm3-1.050g/
cm3, boiling point that reaction generates flashes out less than the reaction light component of cut point, boiled in 40-65m% by arene content
Point is higher than the fraction (hydrogenation tail oil) of the cut point as the raw material for preparing mesophase pitch.It properly increases and cuts in the temperature range
Cutpoint temperature is also advantageous mesophase pitch quality prepared by raising, such as fraction cut point is at 420-450 DEG C.
The considerations of being handled with aforementioned low-sulfur slurry oil is identical, can be by hydrogenation tail oil directly as centre in the embodiment
Asphalt phase prepares raw material, alternatively, the hydrogenation tail oil is mixed in a certain ratio with the extraction light component, is dripped as interphase
Blueness prepares raw material, and mesophase pitch is prepared through thermal polycondensation.Mixed proportion is extraction light component:Hydrogenation tail oil=0%-40%:
100%-60%, and the density of mixed raw material is controlled in 0.970-1.1g/cm3, W metal, the total content of V, Al, Fe, Na and Ca
<2 μ g/g, remaining parameter are handled with aforementioned low-sulfur slurry oil.
Mesophase pitch wide area anisotropic structure ratio prepared by the method for the present invention is high (90% or more), is to prepare height
The quality raw materials of performance Carbon Materials are decoupled by preparing the mesophase pitch with coking, conducive to high-quality is prepared
Oil system needle coke product.
The method of the present invention, through high-temperature calcination (general 1300-1500 DEG C), then carries out quality analysis to obtained needle coke：
The coefficient of thermal expansion of -600 DEG C of room temperature is measured according to petroleum coke MEASURING THE THERMAL EXPANSION COEFFICIENT standard method RIPP 24-90；Using GB/
T6155-2008 measures needle coke real density；Needle coke sulfur content is measured using GB/T24526-2009；It is surveyed using YB/T5189
Determine carbon material fugitive constituent；Ash content is measured using GB/T1429；The test method of resistivity uses GB/T 24521.
Compared to technology used at present, core of the invention effect is：Catalytic cracked oil pulp is after extraction and separation, extraction
Light component and extraction intermediate species are substantially free of asphalitine and solid (ash content), extract intermediate species and extract light component or add
Hydrogen tail oil is mixed in a certain ratio with extraction light component and high-quality mesophase pitch raw material, the density of mesophase pitch raw material can be obtained
In 0.970-1.1g/cm3(more excellent is 1.0-1.1g/cm3), sulfur content<0.4m%, arene content 40m%-65m%, ash content contain
Amount<0.01%, C7 asphalitine<0.1%, W metal, the total content of V, Al, Fe, Na and Ca<5 μ g/g are (more excellent to be<2 μ g/g),
Anisotropic high-quality mesophase pitch is prepared under the conditions of thermal polycondensation appropriate, further by by the mesophase pitch
Preparation and coking process decouple, solve mesophase pitch synthesis and the contradiction in pyrogenetic reaction condition, to obtain Gao Pin
Matter oil system needle coke.
Combined method provided by the invention can not only realize the refined of slurry oil, make full use of catalytic cracked oil pulp, can also obtain
To high-quality mesophase pitch, while thermal polycondensation reaction prepares mesophase pitch and prepares needle coke process point with delayed coking reaction
Do not implement in different device, that is, two processes realize decoupling, do not interfere with each other and influence, more conducively realization of industrialization, also solve
The problem of coking technology controlling and process difficulty in needle coke production, and then the needle coke product of acquisition high-quality.
Explanation：In the case where not providing especially definition, content form of presentation or m% of the present invention are quality
Percentage composition.
The solution of the present invention and effect are further disclosed below in conjunction with specific embodiment, but should not be construed as to the present invention's
It can practical range composition any restrictions.
Embodiment 1
Use certain catalytic cracked oil pulp for raw material, slurry oil property see the table below 1, according to flow implementation shown in FIG. 1.
Lighter hydrocarbons solvent group becomes iso-butane, normal butane accounts for 75m%, 25m% respectively, 139.4 DEG C of pseudocritical temperature, catalysis
Slurry oil enters from extraction tower 1 (the present embodiment is sieve-plate tower) jacking, 120 DEG C of inlet temperature of stabilizer, and solvent is sent into from extraction tower bottom, into tower temperature
80 DEG C of degree, agent oil quality is than 2.5:1, tower pressure interior force 4.5MPa, extractant are extracted with slurry oil raw material through counter current contacting
Knockout tower 2 is sent out from tower top and entered to extracting, the extraction oil phase of formation, and 1 head temperature of tower is 86.2 DEG C, and raffinate phase is then from bottom of tower
Discharge is recycled as raffinate heavy constituent.
1 embodiment of table, 1 slurry oil feedstock property and extraction and separation result
Knockout tower 2 is void tower, extracts 150 DEG C of the inlet temperature of oil phase, the separating pressure 4.35MPa in tower is separated into tower
The light oil phase on top and the heavy oil phase of bottom of tower, light oil mutually enter supercritical solvent recovery tower 3, control tower pressure interior force 4.25MPa, temperature
190 DEG C, solvent density 0.0847g/cm3, become extraction after stripping recycling design by the product containing a small amount of solvent is obtained from bottom
Light component is taken, and the heavy oil of 3 bottom of tower mutually obtains extraction intermediate species through stripping separation solvent.It can be seen by 1 separating resulting of table
To extraction light component 15.0m%, intermediate species 60.1m% is extracted, the impurity content of the two is significantly reduced, ash content<
0.01m%, asphalt content<0.1m%, total metal contents in soil are about 1 μ g/g, and fragrance divides content to be 54.09m%.
Extraction intermediate species is prepared into raw material feeding thermal polycondensation reactor 5 as mesophase pitch, 420 DEG C of temperature, when
Between carry out thermal polycondensation under the conditions of 3h, pressure 1.5MPa mesophase pitch be obtained by the reaction, being re-fed into coke drum, to implement delayed coking anti-
It answers.
As shown in Figure 1, coke drum 6 and 7 rotations use, another is devoked when one of them is for pyrogenetic reaction, that is,
Gained mesophase pitch is alternately sent into coke drum 6 and 7, the coking of 490 DEG C of raw material inlet temperature of stabilizer, pressure 0.3MPa, time 48h
Needle coke is prepared in delayed pyrogenetic reaction under reaction condition, and gained needle coke is calcined through 1300 DEG C, measures it and thermally expands system
The properties such as number (CTE), real density, sulphur (S) content, fugitive constituent, ash content, resistivity and yield, the results are shown in Table 2.
2 embodiment of table, 1 calcined needle coke property
Embodiment 2
Certain catalytic cracked oil pulp is raw material, and property is shown in Table 3, and lighter hydrocarbons solvent group becomes propane, iso-butane, normal butane and accounts for respectively
25m%, 50m%, 25m%, 127.0 DEG C of pseudocritical temperature, extraction and lock out operation flow are the same as embodiment 1, difference
For：Extraction tower 1 is packed tower, and catalytic cracked oil pulp is into 100 DEG C of 1 head temperature of tower, and for solvent into 70 DEG C of 1 bottom temp of tower, agent is oily
Mass ratio 3.5:1, pressure 5.0MPa in tower 1, and measure 75.6 DEG C of the tower top temperature of extraction tower；Knockout tower 2 is packed tower, extraction
135 DEG C of the inlet temperature of oil phase, pressure 4.8MPa in tower 2；Light oil mutually enters supercritical solvent recovery tower 3, pressure in control tower 3
4.7MPa, 180 DEG C of temperature, solvent density 0.107g/cm3。
It can see by 3 extraction and separation result of table, according to extraction light component 20m% obtained by the present embodiment technique, in extraction
Between component 47.8m%, the extraction intermediate species impurity of separation significantly removed, ash content<0.01m%, asphalt content<
0.1m%, total metal are about 4.3 μ g/g, and fragrant part content reaches 45.7m%, sulfur content 0.3m%.
Gained extraction intermediate species is prepared into raw material as mesophase pitch and is sent into thermal polycondensation reactor 5, in temperature 440
DEG C, carry out thermal polycondensation under the conditions of time 4h, pressure 1.0MPa mesophase pitch be obtained by the reaction, be re-fed into coke drum and implement delay coke
Change reaction.
As shown in Figure 1, with embodiment 1, coke drum 6 and 7 rotations use.Gained mesophase pitch is alternately sent into coke drum
6 and 7, under the conditions of 495 DEG C of raw material inlet temperature of stabilizer, pressure 0.7MPa, time 36h delayed pyrogenetic reaction needle coke is prepared,
Gained needle coke is calcined through 1400 DEG C, and the properties such as yield are shown in Table 4.
3 embodiment of table, 3 slurry oil feedstock property and extraction and separation result
4 embodiment of table, 2 calcined needle coke property
Embodiment 3
Certain catalytic cracked oil pulp is raw material, and slurry oil property see the table below 5, and lighter hydrocarbons solvent group becomes normal butane, pentane is distinguished
Account for 85m%, 15m%, 149.5 DEG C of pseudocritical temperature.It extracts and lock out operation flow is with embodiment 1, the difference is that：
Extraction tower 1 is packed tower, and catalytic slurry is into 150 DEG C of 1 head temperature of tower, and solvent is into 120 DEG C of 1 bottom temp of tower, agent oil quality ratio
4.5:1, pressure 6.0MPa in tower 1,124.5 DEG C of the tower top temperature of extraction process；Knockout tower 2 is sieve-plate tower, extracts entering for oil phase
Mouthful 175 DEG C of temperature, pressure 5.8MPa in tower 2；Light oil mutually enters supercritical solvent recovery tower 3, pressure 5.6MPa in control tower 3,
210 DEG C of temperature, solvent density 0.126g/cm3。
It can see by 5 extraction and separation result of table, according to extraction light component 15m%, middle groups obtained by the present embodiment technique
53.5m%, the extraction intermediate species impurity of separation is divided significantly to be removed, ash content 0.03m%, asphalt content 0.2m%,
Total metal is less than 5 μ g/g, and fragrant part content is up to 65.11m%, sulfur content 0.45m%.
Obtained extraction intermediate species is prepared into raw material directly as mesophase pitch and is sent into thermal polycondensation reactor 5,440
DEG C, thermal polycondensation reaction is carried out under the conditions of 4h, 1.0MPa, obtains mesophase pitch, is re-fed into coke drum and is implemented delayed coking reaction.
As shown in Figure 1, with embodiment 1, coke drum 6 and 7 rotations use.Gained mesophase pitch is alternately sent into coke drum
6 and 7, under the conditions of 505 DEG C of raw material inlet temperature of stabilizer, pressure 0.35MPa, time 18h delayed pyrogenetic reaction needle coke is prepared,
Gained needle coke is calcined through 1420 DEG C, and the properties such as yield are shown in Table 6.
5 embodiment of table, 3 slurry oil feedstock property and extraction and separation result
6 embodiment of table, 3 calcined needle coke property
Embodiment 4
The extraction light component that embodiment 3 is obtained is with extraction intermediate species by 15.0:53.5 output quality ratio mixing, as
Mesophase pitch prepares raw material and is sent into thermal polycondensation reactor 5, and heat is carried out under the conditions of 430 DEG C of temperature, time 6h, pressure 0.8MPa
Polycondensation reaction obtains mesophase pitch, is re-fed into coke drum and implements delayed coking reaction.
As shown in Figure 1, with embodiment 1, coke drum 6 and 7 rotations use.Gained mesophase pitch is alternately sent into coke drum
6 and 7, under the conditions of 490 DEG C of raw material inlet temperature of stabilizer, pressure 0.55MPa, time 16h delayed pyrogenetic reaction needle coke is prepared,
Gained needle coke is calcined through 1350 DEG C, and the properties such as yield are shown in Table 7.
7 embodiment of table, 4 calcined needle coke property
Embodiment 5
Certain catalytic cracked oil pulp is raw material, and slurry oil property is shown in Table 8.Add hydrogen de- according to flow implementation shown in FIG. 1 is necessary
Sulphuring treatment.
Lighter hydrocarbons solvent group becomes normal butane, iso-butane, pentane and accounts for 95m%, 4m%, 1m%, pseudocritical temperature respectively
155.2 DEG C, extraction tower 1 is packed tower, and catalytic slurry is into 160 DEG C of 1 head temperature of tower, and solvent is into 130 DEG C of 1 bottom temp of tower, agent
Oil quality is than 4.5:1, pressure 4.3MPa in tower 1 measure 136.0 DEG C of the temperature of extraction tower top；Knockout tower 2 is sieve-plate tower, extraction
155 DEG C of the inlet temperature of oil phase, pressure 4.2MPa in tower 2；Light oil mutually enters supercritical solvent recovery tower 3, pressure in control tower 3
4.1MPa, 180 DEG C of temperature, makes solvent density 0.113g/cm3, obtained overhead product extracts containing a small amount of solvent through overcritical separation
Extraction light component is obtained after taking solvent, the heavy oil of 2 bottom of knockout tower mutually after stripping detaches solvent, obtains extraction intermediate species.
It can see by 8 extraction and separation result of table, according to light component 15.5m% is extracted obtained by the present embodiment technique, extract
Intermediate species 58.0%.Obtained extraction intermediate species is sent into hydrodesulphurisatioreactors reactors 4, is urged using conventional residuum hydrodesulfurization
Agent (γ-Al2O3Load C o and Mo, hole hold 0.4ml/g, aperture 7-13nm, specific surface 150m2/ g) implement hydrodesulfurization processing,
Its hydroprocessing pressure 6.0MPa, hydrogen to oil volume ratio 600:1, air speed 1.0h-1, hydrogenation products are obtained, which is often subtracted
Pressure distillation collects boiling point and is higher than 350 DEG C of hydrogenation tail oil, boiling point less than 350 DEG C plus hydrogen light fraction be then discharged and (can individually make
Collected for byproduct, the light component of reacting that can also be generated with pyrocondensation collecting process merges discharge), it is accounted for through converting hydrogenation tail oil yield
Slurry oil 49.8m% (is shown in Table 8).
Extraction light component is pressed 15.5 with hydrogenation tail oil:The natural yield ratio of 49.8 mass ratioes mixes, and is sent into thermal polycondensation
Reactor 5 carries out thermal polycondensation reaction under the conditions of 450 DEG C of temperature, time 8h, pressure 2.0MPa, obtains mesophase pitch, then send
Enter coke drum and implements delayed coking reaction.
8 embodiment of table, 5 slurry oil feedstock property, extraction and separation and hydrogenation tail oil result
9 embodiment of table, 5 calcined needle coke property
As shown in Figure 1, with embodiment 1, coke drum 6 and 7 rotations use.Gained mesophase pitch is alternately sent into coke drum
6 and 7, delayed coking reaction is carried out under the conditions of 510 DEG C of raw material inlet temperature of stabilizer, pressure 0.45MPa, time 30h, is prepared needle-shaped
Coke, gained needle coke are calcined through 1350 DEG C, and the properties such as yield are shown in Table 9.
Embodiment 6
Catalytic cracked oil pulp raw material, extraction and lock out operation, hydrodesulfurization are handled with embodiment 5, but at hydrodesulfurization
420 DEG C of fraction cut point, obtains the hydrogenation tail oil fraction that boiling point is higher than 420 DEG C when reason gained hydrogenation products Atmospheric vacuum fractionation,
Yield accounts for slurry oil raw material 42.5m%, referring specifically to table 10.
Extraction light component is pressed 15.5 with hydrogenation tail oil:The natural yield ratio of 42.5 mass ratioes mixes, and is sent into thermal polycondensation
Thermal polycondensation reaction occurs under the conditions of 420 DEG C of reaction temperature, reaction time 6h, polycondensation pressure 0.7MPa for reactor 5, in obtaining
Between asphalt phase, be re-fed into coke drum implement delayed coking reaction.
As shown in Figure 1, with embodiment 1, coke drum 6 and 7 rotations use.Gained mesophase pitch is alternately sent into coke drum
6 and 7,500 DEG C of raw material inlet temperature of stabilizer, pressure 0.7MPa, time carry out delayed coking reaction under the conditions of for 24 hours, are prepared needle-shaped
Coke, gained needle coke are calcined through 1450 DEG C, and the properties such as yield are shown in Table 11.
10 embodiment of table, 6 hydrogenation tail oil result
11 embodiment of table, 6 calcined needle coke property
Embodiment 7
Certain catalytic cracked oil pulp is raw material, and slurry oil property is shown in Table 12, and lighter hydrocarbons solvent group becomes normal butane, iso-butane, positive penta
Alkane accounts for 5m%, 3m%, 92m%, 191.7 DEG C of pseudocritical temperature respectively.Extraction tower 1 is packed tower, and catalytic slurry is into the top of tower 1
180 DEG C of temperature, solvent is into 150 DEG C of 1 bottom temp of tower, and agent oil quality is than 4.5:1, pressure 4.0MPa in tower 1, extractant and oil
It starches raw material and realizes extraction through counter current contacting；The extraction oil phase that tower top comes out enters supercritical solvent recovery tower 3, molten through separating and extracting
Obtain extracted component after agent, pressure 3.7MPa in control tower 3,230 DEG C of temperature, solvent density 0.098g/cm3。
12 embodiment of table, 7 slurry oil feedstock property, extraction and separation and hydrogenation tail oil result
13 embodiment of table, 7 calcined needle coke property
It can see by 12 extraction and separation result of table, extracted component 65m%, obtained extraction obtained according to the present embodiment technique
Group is taken to be distributed into hydrodesulphurisatioreactors reactors 4, using conventional residual oil Hydrobon catalyst (γ-Al2O3Load Ni and W metal actives
The catalyst of component, hole hold 0.45ml/g, pore diameter range 8-15nm, specific surface 200m2/ g) implement hydrodesulfurization processing,
Hydroprocessing pressure 10.0MPa, hydrogen to oil volume ratio 800:1, air speed 0.6h-1, hydrogenation products are obtained, which is distilled and is received
Boiling point is taken to be higher than 350 DEG C of hydrogenation tail oil, hydrogenation tail oil yield accounts for slurry oil 61.0m%.
It is sent the hydrogenation tail oil as the raw material for preparing of mesophase pitch into thermal polycondensation reactor 5, in reaction temperature 450
DEG C, thermal polycondensation reaction is carried out under the conditions of time 2h, pressure 1.5MPa, obtain mesophase pitch, be re-fed into coke drum and implement delay
Pyrogenetic reaction.
As shown in Figure 1, with embodiment 1, coke drum 6 and 7 rotations use.Gained mesophase pitch is alternately sent into coke drum
6 and 7,485 DEG C of raw material inlet temperature of stabilizer, pressure 0.35MPa, time under the conditions of for 24 hours delayed pyrogenetic reaction needle coke is prepared,
Gained needle coke is calcined through 1300 DEG C, and the properties such as yield are shown in Table 13.
Claims (11)
1. a kind of separation catalytic cracked oil pulp simultaneously prepares the combined method that oil is needle coke, include the following steps：
Make catalytic cracked oil pulp raw material and extractant counter current contacting in extraction tower, makes the extractant overcritical or sub-
Catalytic cracked oil pulp is extracted under critical condition, forms extraction oil phase and raffinate phase, extraction oil phase is sent into knockout tower
Heating is separated into light oil phase and heavy oil phase, and raffinate phase then obtains raffinate heavy constituent after recovered extractant；
Overcritical separating and extracting solvent is mutually carried out to the light oil, obtains extraction light component, the heavy oil is mutually after detaching solvent
Obtain extraction intermediate species；
The extraction intermediate species or the extraction intermediate species and the mixture of the extraction light component are dripped as interphase
Blueness prepares raw material, carries out thermal polycondensation reaction and mesophase pitch is made, the mass content of the extraction light component in the mixture is not
More than 50%；
Using obtained mesophase pitch, oil system needle coke is prepared using Delayed Coking Technology；
Wherein,
The group of the extractant is divided into C3-C5 light ends fractionations, and its pseudocritical temperature Tc is at 90 DEG C -196 DEG C, the pseudo-critical
Temperature Tc presses formulaIt obtains, x in formulaiIt is the molar fraction of the component i in the light ends fractionation, TciIt is component i
Critical-temperature, n is the number of components contained by the extractant,
Make catalytic cracked oil pulp raw material from extraction tower top into 70-200 DEG C of tower and inlet temperature of stabilizer, extractant is from tower bottom into tower
And 50 DEG C -180 DEG C of inlet temperature of stabilizer, extraction pressure tower are 3.0-10.0MPa, the quality of extractant and catalytic cracked oil pulp raw material
Compare 1.5-5.0:1, the extraction oil phase is isolated from tower top, the raffinate phase is isolated from bottom of tower.
2. separation catalytic cracked oil pulp according to claim 1 simultaneously prepares the combined method that oil is needle coke, wherein will in
Between asphalt phase prepare raw material carry out thermal polycondensation reaction mesophase pitch, reaction pressure 0.1-3.0MPa, reaction temperature 400- is made
490 DEG C, reaction time 3-12h.
3. separation catalytic cracked oil pulp according to claim 1 simultaneously prepares the combined method that oil is needle coke, wherein described
The condition of delayed coking reaction controls：480-510 DEG C of raw material inlet temperature of stabilizer, pressure 0.1-1.0MPa, reaction time 12-36h.
4. separation catalytic cracked oil pulp according to claim 2 simultaneously prepares the combined method that oil is needle coke, wherein described
The condition of delayed coking reaction controls：480-510 DEG C of raw material inlet temperature of stabilizer, pressure 0.1-1.0MPa, reaction time 12-36h.
5. separation catalytic cracked oil pulp according to claim 1 simultaneously prepares the combined method that oil is needle coke, wherein by institute
It states extraction oil heat phase to be warming up to higher than 5-90 DEG C of tower top temperature of extraction, into knockout tower, control separating pressure is 3.0-
10.0MPa, the heavy oil are mutually discharged from bottom of tower, the extraction intermediate species are obtained after detaching solvent, the light oil is mutually from tower
Top separates, and extractant is isolated through overcritical, obtains extraction light component.
6. separation catalytic cracked oil pulp according to claim 1 simultaneously prepares the combined method that oil is needle coke, wherein described
When overcritical separating and extracting solvent, the density of extractant is made to be less than 0.20g/cm3, separating pressure 3.0-10.0MPa, and point
It is not higher than 280 DEG C from temperature control.
7. separation catalytic cracked oil pulp according to claim 5 simultaneously prepares the combined method that oil is needle coke, wherein described
When overcritical separating and extracting solvent, the density of extractant is made to be less than 0.20g/cm3, separating pressure 3.0-10.0MPa, and point
It is not higher than 280 DEG C from temperature control.
8. according to any separation catalytic cracked oil pulps of claim 1-7 and the combined method that oil is needle coke is prepared,
In, sulfur content >=0.5m% of the catalytic cracked oil pulp raw material, the combined method further includes：
By the extraction intermediate species or extracts intermediate species and extract the first hydrogenated desulfurization process of mixture of light component, place
Hydrogenated oil after reason, which be fractionated collecting, adds hydrogen light fraction and hydrogenation tail oil, and fraction cut point is 350-450 DEG C, and boiling point is higher than
Sulfur content≤0.3m% of the hydrogenation tail oil of cut point, density is in 0.970g/cm3-1.050g/cm3, arene content is in 40-
65m%；
The hydrogenation tail oil or the hydrogenation tail oil and the mixture of the extraction light component prepare original as mesophase pitch
Material, the mass content of the extraction light component in the mixture are no more than 40%.
9. separation catalytic cracked oil pulp according to claim 8 simultaneously prepares the combined method that oil is needle coke, wherein described
Hydrodesulfurization processing uses residuum hydrodesulfurization catalyst, hydroprocessing pressure 6-16MPa, hydrogen to oil volume ratio 200:1-1200:
1, air speed 0.2-2.0h-1。
10. separation catalytic cracked oil pulp according to claim 1 simultaneously prepares the combined method that oil is needle coke, wherein institute
The density of catalytic cracked oil pulp is stated in 0.970g/cm3-1.200g/cm3, carbon residue<21.0m%, C7 asphalt content<10.0m%,
Ash content<3.0m%, sulfur content<3.0m%.
11. separation catalytic cracked oil pulp according to claim 1 simultaneously prepares the combined method that oil is needle coke, wherein institute
The mesophase pitch obtained prepares the density of raw material in 0.970-1.1g/cm3, arene content 40m%-65m%, sulfur content<
0.4m%.
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| CN110791315B (en) * | 2019-11-15 | 2022-07-12 | 陕西师范大学 | Method for preparing needle coke by using catalytic cracking slurry oil |
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| CN112812802B (en) * | 2021-01-13 | 2022-04-15 | 中国石油大学(华东) | Continuous process for preparing mesophase pitch by refining raw oil |
| CN115216335A (en) * | 2021-04-14 | 2022-10-21 | 张家港保税区慧鑫化工科技有限公司 | Needle coke production process |
| CN113801689B (en) * | 2021-09-10 | 2022-10-18 | 中海油天津化工研究设计院有限公司 | Method for treating heavy oil by supercritical hydrothermal modification and delayed coking technology |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06158061A (en) * | 1990-12-26 | 1994-06-07 | Nippon Petrochem Co Ltd | Production of oxidation-resistance solvent |
| CN1393525A (en) * | 2001-06-29 | 2003-01-29 | 中国石油化工股份有限公司 | Process for transforming high-sulfur high-metal residual oil |
| CN1410510A (en) * | 2001-09-26 | 2003-04-16 | 石油大学(北京) | Solvent extraction technology for removing high softening point asphalt in petroleum slag and its equipment |
| CN101050383A (en) * | 2007-04-30 | 2007-10-10 | 中国石油化工股份有限公司 | Combined technique for processing heavy oil |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104449840B (en) * | 2014-11-05 | 2017-01-11 | 中国石油大学(北京) | Method for processing low-grade heavy oil |
-
2015
- 2015-03-30 CN CN201510144811.3A patent/CN106147835B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06158061A (en) * | 1990-12-26 | 1994-06-07 | Nippon Petrochem Co Ltd | Production of oxidation-resistance solvent |
| CN1393525A (en) * | 2001-06-29 | 2003-01-29 | 中国石油化工股份有限公司 | Process for transforming high-sulfur high-metal residual oil |
| CN1410510A (en) * | 2001-09-26 | 2003-04-16 | 石油大学(北京) | Solvent extraction technology for removing high softening point asphalt in petroleum slag and its equipment |
| CN101050383A (en) * | 2007-04-30 | 2007-10-10 | 中国石油化工股份有限公司 | Combined technique for processing heavy oil |
Non-Patent Citations (2)
| Title |
|---|
| 催化裂化油浆富芳烃馏分的组成及其炭化行为;李学军等;《石油化工》;20071130;第36卷(第11期);第1104页-1109页 * |
| 催化裂化油浆超临界萃取组分热缩聚生成中间相沥青的定量研究;李春霞等;《石油学报（石油加工）》;20150228;第31卷(第1期);第145-148页 * |
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