CN106929100B - A kind of preparation method of aromatic rubber oil - Google Patents
A kind of preparation method of aromatic rubber oil Download PDFInfo
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- CN106929100B CN106929100B CN201511008851.1A CN201511008851A CN106929100B CN 106929100 B CN106929100 B CN 106929100B CN 201511008851 A CN201511008851 A CN 201511008851A CN 106929100 B CN106929100 B CN 106929100B
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G67/00—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only
- C10G67/02—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only plural serial stages only
- C10G67/04—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only plural serial stages only including solvent extraction as the refining step in the absence of hydrogen
- C10G67/0409—Extraction of unsaturated hydrocarbons
- C10G67/0436—The hydrotreatment being an aromatic saturation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L91/00—Compositions of oils, fats or waxes; Compositions of derivatives thereof
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- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The present invention relates to oil and petroleum distillate manufacture fields, disclose a kind of preparation method of aromatic rubber oil, and this method includes：Feedstock oil is contacted with extraction solvent, obtain raffinate and Extract, after removing solvent, respectively obtain raffinating oil containing few cycloaromatics and the tapped oil containing condensed-nuclei aromatics, tapped oil containing condensed-nuclei aromatics obtains the hydrogenated oil of condensed-nuclei aromatics oil through hydrogenated processing, wherein, refractive index of the hydrogenated oil of the condensed-nuclei aromatics oil obtained through hydrogenated processing at 20 DEG C is 1.5 1.61, the feedstock oil is rich in aromatic naphtha, first part and second part should be contained rich in aromatic naphtha, the first part is the tapped oil and/or catalytic cracking clarified oil of refinery's lube base oil solvent extraction production, the second part is the hydrogenated oil of condensed-nuclei aromatics oil, wherein, the aromatic ring number of few cycloaromatics is one or two, the aromatic ring number of the condensed-nuclei aromatics is three or three or more.The method of the present invention can effectively improve the yield and quality (aromatic carbon content) of environment-friendly type aromatic rubber oil.
Description
Technical field
The present invention relates to a kind of preparation methods of aromatic rubber oil.
Background technology
It is special for the elasticity and the flexibility that improve rubber workability in process of production and easily mixing property and rubber etc.
Property, rubber oil usually is added in the production process of rubber.Rubber oil presses the difference of its chemical composition, is divided into paraffinic, ring
Alkane type and aromatic hydrocarbon rubber oil.Aromatic rubber oil (Distillate Aromatic Extract, be abbreviated as DAE) has virtue
The features such as carbon content is high, density is big, viscosity is high, good with polar rubber compatibility and processing performance is superior, is tire and footwear system
The excellent filler of butadiene-styrene rubber used in product, DAE typically constitute from 30% or so of rubber gross mass.Since butadiene-styrene rubber is butadiene
With the random copolymer of styrene, copolymer side chain carries phenyl ring, and therefore, arene content is higher in butadiene-styrene rubber filling oil, fills out
It is oil-filled better with the high molecular compatibility of butadiene-styrene rubber, the performance improvement of oil-extended rubber it is better.DAE is usually by lubrication oil base
The tapped oil or oil slurry from catalytically cracked heavy oil that feedstock oil is produced through solvent refining unit in plinth oil production technology are through reprocessing or adjusting
Conjunction produces.
From 1 day January in 2010, tire and its accessory into EU market need to instruct 2005/69/EC using it is met
(polycyclic aromatic hydrocarbon content that IP346 methods measure is less than 3% to quality requirement, and benzo (a) pyrene content is not more than 1mg/kg, benzo (a)
Anthracene, in the wrong, benzo (b) fluoranthene, benzo (k) fluoranthene, benzo (j) fluoranthene, benzo (a) anthracene, benzo (e) anthracene and dibenzo (a, h) anthracene
Eight kinds of condensed-nuclei aromatics total contents are not more than 10mg/kg) the production of filling oil, the U.S. and Japanese also make similar production in succession
The quality standard of tire filling oil.China's tyre industry is typical export-oriented industry, and about 45% tire product exports Europe
Alliance or the U.S., therefore, above-mentioned country have seriously affected China's tyre industry to the raising of rubber filling oil quality standard
Export business.
Currently, China has more scientific researches or production unit develops the production tire use for meeting European Union environmental protection index request
The oily patented technology of filling.CN102453538A discloses a kind of production method of environmentally friendly tyre aromatic oil, and this method is to moisten
Lubricating oil solvent refining tapped oil be raw material, feedstock oil through hydrogenated processing after, the hydrotreating oil of raw material is produced through solvent extraction again
Tire environment-friendly rubber oil.Although this method is referred to using suitable catalyst for hydro-upgrading and right under conditions of opposite mitigation
Feedstock oil carries out plus hydrogen, can reduce aromatic hydrocarbons loss, still, be made full use of from aromatic rubber oil control of product quality and resource
For in angle, the production method of the aromatic naphtha of the prior art still has larger room for improvement.
Invention content
The purpose of the present invention is overcome aromatic rubber oil control of product quality difference in the prior art and cannot make full use of
The defect of petroleum resources and environment-friendly type aromatic rubber oil yield and quality can be improved by providing one kind, and can make full use of stone
The aromatic rubber oil preparation method of oily resource.
To achieve the goals above, the present invention provides a kind of preparation method of aromatic rubber oil, and this method includes：By raw material
Oil is contacted with extraction solvent, obtains raffinate and Extract, after removing solvent, respectively obtain containing lack cycloaromatics raffinating oil with
Tapped oil containing condensed-nuclei aromatics, the tapped oil containing condensed-nuclei aromatics obtain the hydrogenated oil of condensed-nuclei aromatics oil through hydrogenated processing,
In, the refractive index of the hydrogenated oil of the condensed-nuclei aromatics oil obtained through hydrogenated processing at 20 DEG C is 1.5-1.61, and the feedstock oil is
Rich in aromatic naphtha, first part and second part should be contained rich in aromatic naphtha, the first part is refinery's lube base oil
The tapped oil and/or catalytic cracking clarified oil of solvent extraction production, the second part are the hydrogenated oil of condensed-nuclei aromatics oil,
Wherein, the aromatic ring number of few cycloaromatics is one or two, the aromatic ring number of the condensed-nuclei aromatics be three or three with
On.
CN102453538A discloses a kind of production method of environmentally friendly tyre aromatic oil, and this method includes by feedstock oil
(furfural extract oil) plus hydrogen, and the hydrogenated oil of feedstock oil is prepared into environment-friendly type aromatic hydrocarbon rubber extender oil through solvent extraction.This method
Although referring to that feedstock oil hydroconversion condition mitigates, aromatic hydrocarbons loss can be reduced, there is no the hydrogenation reaction degree for proposing feedstock oil
Influence to end product quality, and the extraction that this method extracts the hydrotreating oil solvent for still containing the single double ring arene in part
Oil (condensed-nuclei aromatics oil) is expelled directly out device, is unfavorable for making full use of for petroleum resources.
The present invention uses the tapped oil produced containing refinery's lube base oil solvent extraction and/or catalytic cracking clarification
The mixture of the hydrogenated oil of the condensed-nuclei aromatics oil obtained after the Extract removal solvent that solvent extraction produces in oil and the present invention
Make feedstock oil, feedstock oil obtains making environment-friendly type aromatic hydrocarbon rubber extender oil containing few raffinating oil for cycloaromatics through solvent extraction, contain
The tapped oil of condensed-nuclei aromatics makees the raw material of hydrogenation plant, and adds hydrogen after hydrogenated by tapped oil of the control containing condensed-nuclei aromatics
The refractive index of oil, can best limit by environmental-friendly rubber filling oil undesirable components tricyclic in the tapped oil containing condensed-nuclei aromatics and
Aromatic hydrogenation saturation more than tricyclic is converted into the oily ideal composition of the filling such as monocycle or double ring arene, and then effectively improves environment-friendly type
The quality (CA values) and yield of rubber filling oil.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Description of the drawings
Attached drawing is to be used to provide further understanding of the present invention, an and part for constitution instruction, with following tool
Body embodiment is used to explain the present invention together, but is not construed as limiting the invention.In the accompanying drawings：
Fig. 1 is a kind of schematic flow diagram of the preparation of the aromatic rubber oil of preferred embodiment of the present invention.
Reference sign
1 raw material oil pipeline；2 first static mixers；3 feedstock oils detect and control device；
4 pre-treatment solvents pipelines；5 mixed raw material pipelines；6 second static mixers；
7 extraction device raw material oil pipelines；8 solvent extraction apparatus；9 raffinate oil out tubulature line；
10 hydrogenation plant raw material oil pipelines；11 hydrogenation plants；12 hydrogenated oil detection devices；
13 hydrogenated oil pipeloops.
Specific implementation mode
The specific implementation mode of the present invention is described in detail below.It should be understood that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
According to the present invention, the preparation method of the aromatic rubber oil includes：Feedstock oil is contacted with extraction solvent, is taken out
Extraction raffinate and Extract after removing solvent, respectively obtain raffinating oil containing few cycloaromatics and the tapped oil containing condensed-nuclei aromatics, contain
There is the tapped oil of condensed-nuclei aromatics to obtain the hydrogenated oil of condensed-nuclei aromatics oil through hydrogenated processing, wherein the condensed ring obtained through hydrogenated processing
Refractive index of the hydrogenated oil of aromatic naphtha at 20 DEG C is 1.5-1.61, and the feedstock oil is that should be rich in aromatic naphtha rich in aromatic naphtha
Containing first part and second part, the first part be refinery's lube base oil solvent extraction production tapped oil and/
Or catalytic cracking clarified oil, the second part are the hydrogenated oil of condensed-nuclei aromatics oil, wherein the aromatic ring of few cycloaromatics
Number is one or two, and the aromatic ring number of the condensed-nuclei aromatics is three or three or more.
The tapped oil (condensed-nuclei aromatics oil) that feedstock oil is produced through solvent extraction is to be mainly containing tricyclic and the above aromatic hydrocarbons of tricyclic
Main material is the undesirable components of environmentally-frierubber rubber filling oil, (the environment-friendly type virtue of raffinating oil that feedstock oil is produced through solvent extraction
Hydrocarbon rubbers oil) be mainly contain monocycle and it is bicyclic based on material, be the ideal composition of environmentally-frierubber rubber filling oil.
It was found by the inventors of the present invention that the depth of the hydrogenation reaction of tapped oil of the control containing condensed-nuclei aromatics, it can be by three
Aromatic hydrogenation more than ring and tricyclic is converted into environmentally-frierubber rubber filling oil ideal composition list double ring arene, and can prevent excessively
Add hydrogen saturation to be converted into cycloalkane, and leads to the reduction of product aromatic carbon content.
The present inventor it has furthermore been found that refractive index be not it is directly related with the content of oil product aromatic hydrocarbons, but with oil
The carbon type of hydrocarbon has certain incidence relation in product.Inventor has found that aromatic carbon content (CA%) is higher, and condensed-nuclei aromatics oil adds hydrogen
The refractive index of oil is higher；Cycloalkanes carbon content (CN%) and alkane carbon content (CP%) are higher, the hydrogenated oil of condensed-nuclei aromatics oil
Refractive index is lower.Therefore, by controlling the hydrogenation reaction degree of the tapped oil containing condensed-nuclei aromatics, after keeping its hydrogenated plus hydrogen
The refractive index of oil is within the scope of the invention namely refractive index is 1.5-1.61, and tricyclic and the above aromatic hydrocarbons of tricyclic both may be implemented
Add hydrogen saturation for single double ring arene, but can be to avoid causing product aromatic carbon content to reduce because of excessive hydrogenation saturated reaction the problem of.
Further preferably, control plus hydrogen degree make the hydrogenated oil of the condensed-nuclei aromatics obtained through hydrogenated processing oil at 20 DEG C
Refractive index be 1.52-1.6 can be better achieved the present invention goal of the invention.
According to the present invention, through solvent extraction and the tapped oil (condensed-nuclei aromatics oil) that is obtained after solvent detaches by plus hydrogen at
The hydrogenated oil of the condensed-nuclei aromatics oil obtained after reason can feed directly as the second part of feedstock oil and feed one with first part
It rises and carries out solvent extraction step.Therefore, the refining ratio of mixing of first part and second part is not particularly limited, can be according to equipment
Processing capacity and select the inlet amount of first part appropriate and second part.
According to the present invention, the feedstock oil is rich in aromatic naphtha, and the second part that should contain rich in aromatic naphtha comes from this
The tapped oil obtained after Extract removal solvent in method by feedstock oil after solvent extraction obtains condensed ring through hydrogenated processing
The hydrogenated oil of aromatic naphtha.Solvent extraction system is recycled back to as raw material using the hydrogenated oil of condensed-nuclei aromatics oil as rich in aromatic naphtha
Oil, can be by monocycle of the condensed-nuclei aromatics oil after adding hydrogen in gained hydrogenation products, double ring arene again by solvent extraction mistake
Journey and separate, and as target product environment-friendly aromatic rubber oil, so improve environment-friendly type aromatic rubber oil yield and
Aromatic carbon content, and improve the economic use value of the hydrogenated oil of condensed-nuclei aromatics oil.
According to the present invention, as long as condensed-nuclei aromatics oil is taken out by adding the condensed-nuclei aromatics hydrogenated oil that hydrogen obtains to return as solvent
Propose the charging of system, you can improve the yield of environment-friendly type aromatic rubber oil and the purpose of aromatic carbon content to realize.Preferable case
Under, the hydrogenated oil of whole condensed-nuclei aromatics oil is returned into one of the charging as solvent extraction system, so that condensed-nuclei aromatics oil adds
The oily ideal composition of the filling such as monocycle, double ring arene in hydrogen oil enters in final environment-friendly rubber oil product component.
According to the present invention, the extraction solvent usually contains main solvent and secondary solvent, using the gross mass of extraction solvent as base
The content of standard, secondary solvent can be 0.2-10 weight %, and the content of main solvent can be 90-99.8 weight %, it is preferable that secondary solvent
Content be 1-8 weight %, the content of main solvent is 92-99 weight %.
According to the present invention, the mass ratio of the hydrogenated oil of extraction solvent and feedstock oil can be 0.5:1 to 6:1, preferably 1:1
To 4:1.By controlling the mass ratio of feedstock oil and extraction solvent within the scope of aforementioned proportion, the original can be better achieved
Tricyclic and the above aromatic hydrocarbons of tricyclic and list double ring arene and alkane is sufficiently separated in material oil.
According to the present invention, the extraction solvent usually contains main solvent and secondary solvent, wherein main solvent can be this field
Conventional main solvent.Under preferable case, the main solvent is in furfural, phenol, dimethyl sulfoxide (DMSO) and N-Methyl pyrrolidone
It is one or more.The pair solvent can be the secondary solvent of this field routine.Under preferable case, it is described pair solvent be selected from water,
It is one or more in low-carbon alcohols and low-carbon ketone；The low-carbon alcohols are the one or more of the fatty alcohol that carbon atom number is 1-8, into
One step is preferred, and the low-carbon alcohols are one or more in ethyl alcohol, isopropanol, normal propyl alcohol, n-butanol and n-hexyl alcohol；It is described low
Carbon ketone is that carbon atom number is the alkenolic one or more of 3-6, further preferably, the low-carbon ketone be selected from butanone, pentanone and
It is one or more in hexanone.
According to the present invention, under preferable case, before contacting feedstock oil with extraction solvent, this method further includes by raw material
Oil is mixed with pre-treatment solvents, to realize the purpose for reducing feedstock oil viscosity.The pre-treatment solvents usually contain main solvent and
Secondary solvent, on the basis of the gross mass of pre-treatment solvents, the content of secondary solvent is more than 0 weight % to less than or equal to 8 weights
% is measured, the content of main solvent is more than or equal to 92 weight % to less than 100 weight %, further preferably, the content of secondary solvent
Content for 1-4 weight %, main solvent is 96-99 weight %.
According to the present invention, the mixing of the feedstock oil and pre-treatment solvents can be with various mixing apparatus known in the art
Middle progress can also carry out for example, can be carried out in static mixer in the dynamic mixer with agitating paddle.
According to the present invention, the mass ratio of the pre-treatment solvents and feedstock oil can be 0.02:1 to 0.5:1, preferably
0.05:1 to 0.3:1.By mixing feedstock oil within the scope of aforementioned proportion with pre-treatment solvents, can be better achieved described
The above aromatic hydrocarbons of tricyclic and tricyclic in feedstock oil and single double ring arene and alkane are sufficiently separated.
The type selection of main solvent and secondary solvent in the pre-treatment solvents is usually molten with the master in extraction solvent respectively
Agent is identical with the secondary type selection of solvent, it is further preferred that the main solvent and pair solvent in pre-treatment solvents respectively in extraction solvent
Main solvent it is identical with secondary solvent.
According to the present invention, feedstock oil or feedstock oil are contacted with the mixture of pre-treatment solvents with extraction solvent carry out it is molten
Agent extracting carries out in extraction tower.This method includes：By the mixture and extracting of feedstock oil or feedstock oil and pre-treatment solvents
Solvent comes into full contact in extraction tower, obtains raffinate by extracting column overhead, is detached by solvent, pumping is isolated from raffinate
Excess oil (aromatic rubber oil) obtains Extract from extraction tower bottom of tower, is detached by solvent, tapped oil is isolated from Extract
(condensed-nuclei aromatics oil).The extracting column overhead temperatures can be 45 DEG C to 120 DEG C, preferably 50 DEG C to 90 DEG C, the extraction tower
Column bottom temperature can be 35 DEG C to 95 DEG C, preferably 40 DEG C to 80 DEG C.
According to the present invention, as long as after the condition guarantee that the tapped oil containing condensed-nuclei aromatics is carried out to hydrotreating is hydrogenated
The refractive index of the hydrogenated oil of the condensed-nuclei aromatics oil arrived is 1.5-1.61, under preferable case, the condensed-nuclei aromatics oil that is obtained after hydrogenated
Hydrogenated oil refractive index be 1.52-1.6.
According to the present invention, the condition that the tapped oil containing condensed-nuclei aromatics is carried out to hydrotreating generally includes hydrogen point
Pressure, air speed and hydrogenation temperature, under preferable case, hydrogen partial pressure 2-24MPa, air speed 0.1-2h-1, hydrogenation temperature 280-380
DEG C, further preferably, hydrogen partial pressure 6-18MPa, air speed 0.5-1.2h-1, hydrogenation temperature is 300-350 DEG C.
According to the present invention, it is this field institute that the tapped oil containing condensed-nuclei aromatics, which is carried out hydrogenation catalyst used by adding hydrogen,
Well known various Hydrobon catalysts, the hydrogenation catalyst include the active component of carrier and load on this carrier.Institute
It can be the various carriers in existing Hydrobon catalyst to state carrier, for example, can be in amorphous silicon aluminum oxide
It is one or more.The active component of the hydrogenation catalyst can be in Mo, Ni, Co and W one or more, preferably Ni
And/or Mo, most preferably, the hydrogenation catalyst be contain Ni and Mo as the RCS-31 hydrogenation catalysts of active component and/or
Make the RL-2 hydrogenation catalysts of active component containing Ni, W, Mo.The preparation of the hydrogenation catalyst can refer to art technology
The preparation method of Hydrobon catalyst in the prior art well known to personnel, can also be commercially available, for example, described contain Ni
The RL-2 hydrogenation catalysts for making active component as the RCS-31 hydrogenation catalysts of active component and containing Ni, W, Mo with Mo are equal
Commercially available from Sinopec catalyst branch.
In the present invention, the feedstock oil is that should be lubricated rich in the first part that aromatic naphtha contains, refinery rich in aromatic naphtha
The tapped oil of oil base oil solvent extraction production refers to the profit of the second line of distillation of crude oil, the line that subtracts three, the line that subtracts four or frivolous coal tar
The second line of distillation of the dewaxed oil and crude oil of lubricating oil solvent refining tapped oil and lubex, subtracts the line that subtracts three
It is one or more in the solvent refining tapped oil of the dewaxed oil of four lines or frivolous coal tar.
Below in conjunction with attached drawing 1, illustrate a kind of preparation of the aromatic rubber oil of preferred embodiment of the present invention.
It is rich in aromatic naphtha from raw material oil pipeline 1：The tapped oil of refinery lube base oil solvent extraction production and/or
After catalytic cracking clarified oil is mixed with the hydrogenated oil from the condensed-nuclei aromatics of hydrogenated oil pipeline 13 oil in pipeline, through the first static state
Mixer 2 is sufficiently mixed (feedstock oil detection and control device 3 can be used for regulating and controlling two kinds of flows fed), then through locating with from pre-
The pre-treatment solvents of solvent line 4 are managed after the mixing of mixed raw material pipeline 5, are uniformly mixed through the second static mixer 6, through extracting
Device raw material oil pipeline 7 enters solvent extraction apparatus 8, and counter current contacting, raffinate pass through in solvent extraction apparatus 8 with extraction solvent
After solvent recovery removes solvent, through 9 discharger of tubulature line of raffinating oil out, aromatic rubber oil is obtained, Extract is through solvent recovery
Tapped oil (condensed-nuclei aromatics oil) is obtained after removal solvent, the hydrogenated device raw material oil pipeline 10 of condensed-nuclei aromatics oil enters hydrogenation plant
11, after the hydrogenated oily detection of detection device 12 of hydrogenated oil of condensed-nuclei aromatics oil, then hydrogenated oil circulating pipe line 13 returns to feedstock oil.
Attached drawing does not indicate raffinate and Extract solvent recovering system.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail can carry out a variety of simple variants to technical scheme of the present invention within the scope of the technical concept of the present invention, this
A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to it is various can
The combination of energy no longer separately illustrates.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should also be regarded as the disclosure of the present invention.
The present invention will be described in detail by way of examples below.
In following embodiment, hydrogenated oil refractive index is measured by SH/T0724 methods, the aromatic carbon of environment-friendly type aromatic rubber oil
Content is measured by ASTM D2140 methods, and the polycyclic aromatic hydrocarbon content of environment-friendly type aromatic rubber oil passes through 0838 methods of NB/SH/T
It measures, eight kinds of condensed-nuclei aromatics total contents such as benzo (a) the pyrene content of environment-friendly type aromatic rubber oil and benzo (a) pyrene pass through SN/T
1877.3 method measures.
Environment-friendly type aromatic rubber oil (is raffinated oil) calculation formula of yield：Yield %=(solvent extraction raffinate oil × 100)/
Solvent extraction feedstock oil (first part containing feedstock oil and feedstock oil second part).
Embodiment 1
The present embodiment is used to illustrate the preparation of aromatic rubber oil provided by the invention.
First part is the solvent refining tapped oil of crude oil second line of distillation dewaxed oil in feedstock oil, and property is shown in Table 1.
The tapped oil of first part's second line of distillation dewaxed oil is mixed with the hydrogenated oil of second part condensed-nuclei aromatics oil in feedstock oil
Afterwards, then with pre-treatment solvents mix, and in extraction tower with extraction solvent counter current contacting, the master of pre-treatment solvents and extraction solvent
Solvent is N-Methyl pyrrolidone, and secondary solvent is isopropanol, and secondary solvent content is the 3% of each solvent total weight, main
The content of solvent is the 97% of each solvent total weight.The mass ratio of pre-treatment solvents and feedstock oil is 0.1:1, extraction solvent
Mass ratio with feedstock oil is 3.5:1, it is respectively 80 DEG C and 50 DEG C to extract column overhead and column bottom temperature.It is taken out from the tower top of extraction tower
Raffinate oil (environment-friendly type aromatic rubber oil) is isolated in extraction raffinate, and tapped oil (condensed ring is isolated from the Extract of extraction tower bottom of tower
Aromatic naphtha), raffinate oil yield and property are shown in Table 2.
It carries out the tapped oil obtained after solvent detaches by bottom of tower after above-mentioned solvent extraction (condensed-nuclei aromatics oil) to add hydrogen
Reason, hydrotreating catalyst are the RL-2 hydrogenation catalysts of Sinopec catalyst branch production, hydrogen partial pressure 12MPa, volume
Air speed 1.2h-1, the refractive index of 315 DEG C of hydrogenation plant feedstock inlet temperature, the hydrogenated oil of condensed-nuclei aromatics oil is shown in Table 2, gained condensed ring
The hydrogenated oil of aromatic naphtha is fed as the second part of feedstock oil.
Comparative example 1
This comparative example is used to illustrate the preparation of the aromatic rubber oil of reference method.
Using feedstock oil same as Example 1, identical hydrotreating catalyst and identical solvent composition and it is molten
Agent extraction conditions, unlike, hydrogen partial pressure 17MPa, volume space velocity 0.5h-1, 355 DEG C of hydrogenation plant feedstock inlet temperature, control
20 DEG C of refractive index of the hydrogenated oil of obtained condensed-nuclei aromatics oil are 1.4915.20 DEG C of refractive index of hydrogenated oil of condensed-nuclei aromatics oil,
(environment-friendly type aromatic rubber oil) property of raffinating oil is shown in Table 2.
Comparative example 2
This comparative example is used to illustrate the preparation of the aromatic rubber oil of reference method.
Using feedstock oil same as Example 1, identical hydrotreating catalyst and identical solvent composition and it is molten
Agent extraction conditions, unlike, hydrogen partial pressure 2MPa, volume space velocity 2.5h-1, 270 DEG C of hydrogenation plant feedstock inlet temperature controls
20 DEG C of refractive index of the hydrogenated oil of the condensed-nuclei aromatics oil arrived are 1.6217.Hydrogenated oil 20 DEG C of refractive index, raffinates of condensed-nuclei aromatics oil
Oily (environment-friendly type aromatic rubber oil) property is shown in Table 2.
Embodiment 2
The present embodiment is used to illustrate the preparation of aromatic rubber oil provided by the invention.
First part is the dewaxed oil of the crude oil line tapped oil that subtracts three in feedstock oil, and property is shown in Table 1.
The dewaxed oil of first part's line tapped oil that subtracts three is mixed with the hydrogenated oil of second part condensed-nuclei aromatics oil in feedstock oil
Afterwards, then with pre-treatment solvents mix, and in extraction tower with extraction solvent counter current contacting, the master of pre-treatment solvents and extraction solvent
Solvent is phenol, and secondary solvent is pentanone, and secondary solvent content is the 2% of each solvent total weight, and the content of main solvent is equal
It is the 98% of each solvent total weight.The mass ratio of pre-treatment solvents and feedstock oil is 0.3:1, the matter of extraction solvent and feedstock oil
Amount is than being 5:1, it is respectively 95 DEG C and 80 DEG C to extract column overhead and column bottom temperature.Pumping is isolated from the tower top raffinate of extraction tower
Excess oil (environment-friendly type aromatic rubber oil) isolates tapped oil (condensed-nuclei aromatics oil) from the Extract of extraction tower bottom of tower, raffinates oil
Yield and property are shown in Table 2.
It carries out the tapped oil obtained after solvent detaches by bottom of tower after above-mentioned solvent extraction (condensed-nuclei aromatics oil) to add hydrogen
Reason, hydrotreating catalyst are the RL-2 hydrogenation catalysts of Sinopec catalyst branch production, hydrogen partial pressure 6MPa, volume sky
Fast 0.5h-1, 340 DEG C of hydrogenation plant feedstock inlet temperature, the refractive index of the hydrogenated oil of condensed-nuclei aromatics oil is shown in Table 2, gained condensed ring virtue
The hydrogenated oil of hydrocarbon ils is fed as the second part of feedstock oil.
Embodiment 3
The present embodiment is used to illustrate the preparation of aromatic rubber oil provided by the invention.
First part is the tapped oil of the crude oil line that subtracts four in feedstock oil, and property is shown in Table 1.
After first part's line tapped oil that subtracts four is mixed with the hydrogenated oil of second part condensed-nuclei aromatics oil in feedstock oil, then in advance
Solvent mixing is handled, and is with extraction solvent counter current contacting, the main solvent of pre-treatment solvents and extraction solvent in extraction tower
Furfural, secondary solvent are water, and secondary solvent content is the 1% of each solvent total weight, and the content of main solvent is each solvent
The 99% of total weight.The mass ratio of pre-treatment solvents and feedstock oil is 0.5:1, the mass ratio of extraction solvent and feedstock oil is 1.5:
1, it is respectively 70 DEG C and 60 DEG C to extract column overhead and column bottom temperature.(ring of raffinating oil is isolated from the tower top raffinate of extraction tower
Guarantor's type aromatic rubber oil), tapped oil (condensed-nuclei aromatics oil), raffinate oil yield and property are isolated from the Extract of extraction tower bottom of tower
Matter is shown in Table 2.
It carries out the tapped oil obtained after solvent detaches by bottom of tower after above-mentioned solvent extraction (condensed-nuclei aromatics oil) to add hydrogen
Reason, hydrotreating catalyst are the RL-2 hydrogenation catalysts of Sinopec catalyst branch production, hydrogen partial pressure 8MPa, volume sky
Fast 0.8h-1, 320 DEG C of hydrogenation plant feedstock inlet temperature, the refractive index of the hydrogenated oil of condensed-nuclei aromatics oil is shown in Table 2, gained condensed ring virtue
The hydrogenated oil of hydrocarbon ils is fed as the second part of feedstock oil.
Embodiment 4
The present embodiment is used to illustrate the preparation of aromatic rubber oil provided by the invention.
First part is the dewaxed oil of the frivolous coal tar tapped oil of crude oil in feedstock oil, and property is shown in Table 1.
The hydrogenated oil of the dewaxed oil of the frivolous coal tar tapped oil of first part and second part condensed-nuclei aromatics oil in feedstock oil
After mixing, then mix with pre-treatment solvents, and in extraction tower with extraction solvent counter current contacting, pre-treatment solvents and extraction solvent
Main solvent be dimethyl sulfoxide (DMSO), secondary solvent is n-hexyl alcohol, and secondary solvent content is the 8% of each solvent total weight, main
The content of solvent is the 92% of each solvent total weight.The mass ratio of pre-treatment solvents and feedstock oil is 0.2:1, extraction solvent
Mass ratio with feedstock oil is 2.5:1, it is respectively 120 DEG C and 90 DEG C to extract column overhead and column bottom temperature.From the tower top of extraction tower
Raffinate oil (environment-friendly type aromatic rubber oil) is isolated in raffinate, it is (thick to isolate tapped oil from the Extract of extraction tower bottom of tower
Cyclophane hydrocarbon ils), raffinate oil yield and property are shown in Table 2.
It carries out the tapped oil obtained after solvent detaches by bottom of tower after above-mentioned solvent extraction (condensed-nuclei aromatics oil) to add hydrogen
Reason, hydrotreating catalyst are the RCS-31 hydrogenation catalysts of Sinopec catalyst branch production, hydrogen partial pressure 18MPa, body
Product air speed 1.5h-1, the refractive index of 350 DEG C of hydrogenation plant feedstock inlet temperature, the hydrogenated oil of condensed-nuclei aromatics oil is shown in Table 2, and gained is thick
The hydrogenated oil of cyclophane hydrocarbon ils is fed as the second part of feedstock oil.
Embodiment 5
The present embodiment is used to illustrate the preparation of aromatic rubber oil provided by the invention.
First part is catalytic cracking clarified oil in feedstock oil, and property is shown in Table 1.
After first part's catalytic cracking clarified oil is mixed with the hydrogenated oil of second part condensed-nuclei aromatics oil in feedstock oil, then with
Pre-treatment solvents mix, and with extraction solvent counter current contacting in extraction tower, the main solvent of pre-treatment solvents and extraction solvent is equal
For furfural, secondary solvent is ethyl alcohol, and secondary solvent content is the 5% of each solvent total weight, and the content of main solvent is respective
The 95% of solvent total weight.The mass ratio of pre-treatment solvents and feedstock oil is 0.4:1, the mass ratio of extraction solvent and feedstock oil is
5:1, it is respectively 75 DEG C and 70 DEG C to extract column overhead and column bottom temperature.It isolates and raffinates oil from the tower top raffinate of extraction tower
(environment-friendly type aromatic rubber oil) isolates tapped oil (condensed-nuclei aromatics oil), raffinate oil yield from the Extract of extraction tower bottom of tower
And property is shown in Table 2.
It carries out the tapped oil obtained after solvent detaches by bottom of tower after above-mentioned solvent extraction (condensed-nuclei aromatics oil) to add hydrogen
Reason, hydrotreating catalyst are the RCS-31 hydrogenation catalysts of Sinopec catalyst branch production, hydrogen partial pressure 20MPa, body
Product air speed 2.0h-1, the refractive index of 370 DEG C of hydrogenation plant feedstock inlet temperature, the hydrogenated oil of condensed-nuclei aromatics oil is shown in Table 2, and gained is thick
The hydrogenated oil of cyclophane hydrocarbon ils is fed as the second part of feedstock oil.
Embodiment 6
The present embodiment is used to illustrate the preparation of aromatic rubber oil provided by the invention.
First part in feedstock oil same as Example 1 is used to be extracted out for the solvent refining of crude oil second line of distillation dewaxed oil
Oil, identical hydrotreating catalyst and hydroconversion condition and identical solvent composition and solvent extraction condition, unlike,
Before feedstock oil to be contacted to progress solvent extraction with extraction solvent, feedstock oil is not mixed with pre-treatment solvents, and directly will
Feedstock oil is contacted with extraction solvent.20 DEG C of refractive index of the hydrogenated oil of obtained condensed-nuclei aromatics oil, (environment-friendly type aromatic hydrocarbons rubber of raffinating oil
Glue oil) yield and property be shown in Table 2.
Embodiment 7
The present embodiment is used to illustrate the preparation of aromatic rubber oil provided by the invention.
First part in feedstock oil same as Example 1 is used to be extracted out for the solvent refining of crude oil second line of distillation dewaxed oil
Oil, identical hydrotreating catalyst and hydroconversion condition and identical solvent extraction condition, unlike, extraction solvent and
Secondary solvent is free of in pre-treatment solvents.20 DEG C of refractive index of the hydrogenated oil of obtained condensed-nuclei aromatics oil, (environment-friendly type virtue of raffinating oil
Hydrocarbon rubbers oil) yield and property be shown in Table 2.
Embodiment 8
The present embodiment is used to illustrate the preparation of aromatic rubber oil provided by the invention.
Use first part in feedstock oil same as Example 3 for the tapped oil of the crude oil line that subtracts four, at identical plus hydrogen
Reason catalyst, identical solvent extraction condition, unlike, the hydrogen partial pressure of hydrotreater is 2MPa, volume space velocity 1.2h-1, 280 DEG C of hydrogenation plant feedstock inlet temperature.20 DEG C of refractive index of the hydrogenated oil of obtained condensed-nuclei aromatics oil, (environmental protection of raffinating oil
Type aromatic rubber oil) yield and property be shown in Table 2.
Table 1
Table 2
* environment-friendly type aromatic rubber oil (is raffinated oil) calculation formula of yield：Yield %=(solvent extraction raffinates oil ×
100)/solvent extraction feedstock oil (first part containing feedstock oil and feedstock oil second part).
Continued 2
* environment-friendly type aromatic rubber oil (is raffinated oil) calculation formula of yield：Yield %=(solvent extraction raffinates oil ×
100)/solvent extraction feedstock oil (first part containing feedstock oil and feedstock oil second part).
By the yield and aromatic carbon of the embodiment 1 and the environment-friendly type aromatic rubber oil of comparative example 1 and comparative example 2 listed in table 2
The data of content are it is found that if the refractive index of the hydrogenated device production hydrogenated oil of condensed-nuclei aromatics oil exceeds model of the presently claimed invention
It encloses, although environment-friendly type aromatic rubber oil yield (comparative example 1) or environment-friendly type aromatic rubber oil aromatic carbon content (comparative example 2) are slightly
Height, but the corresponding aromatic carbon content of environment-friendly type aromatic rubber oil or yield reduce, that is, comparative example 1 and 2 can not take into account environment-friendly type virtue
Hydrocarbon rubbers oil yield and aromatic carbon content are excellent, and method using the present invention can be then taken into account both well with higher ring
Guarantor's type aromatic rubber oil yield has preferable aromatic carbon content again.
The environment-friendly type aromatic rubber oil yield of embodiment 1, embodiment 6 and embodiment 7 and aromatic carbon content the result shows that, it is former
During material oil produces environment-friendly type aromatic rubber oil through solvent extraction method, extraction solvent contains to be added in secondary solvent or extracting raw material
Pre-treatment solvents can further increase the yield and its aromatic carbon content of environment-friendly type aromatic rubber oil.
The environment-friendly type aromatic rubber oil yield of embodiment 3 and embodiment 8 and aromatic carbon content the result shows that, control is hydrogenated
Refractive index of the hydrogenated oil of obtained condensed-nuclei aromatics oil at 20 DEG C is handled in the preferred range, in environment-friendly type aromatic hydrocarbons rubber
In the case of glue oil aromatic carbon content is comparable, the yield of environment-friendly type aromatic rubber oil can be improved.
Embodiment 2-5 further proves the mixed rich in aromatic naphtha and condensed-nuclei aromatics oil hydrogenated oil of refinery secondary operation production
The environment-friendly type aromatic rubber oil production for meeting environmentally friendly index request in European Union 2005/69/EC instructions can be produced through this method by closing object
Product.
Claims (17)
1. a kind of preparation method of aromatic rubber oil, this method include：Feedstock oil is contacted with extraction solvent, obtain raffinate and
Extract after removing solvent, respectively obtains raffinating oil containing few cycloaromatics and the tapped oil containing condensed-nuclei aromatics, contains condensed ring
The tapped oil of aromatic hydrocarbons obtains the hydrogenated oil of condensed-nuclei aromatics oil through hydrogenated processing, which is characterized in that
Refractive index of the hydrogenated oil of the condensed-nuclei aromatics oil obtained through hydrogenated processing at 20 DEG C is 1.5-1.61, and the feedstock oil is
Rich in aromatic naphtha, first part and second part should be contained rich in aromatic naphtha, the first part is refinery's lube base oil
The tapped oil and/or catalytic cracking clarified oil of solvent extraction production, the second part are the hydrogenated oil of condensed-nuclei aromatics oil,
Wherein, the aromatic ring number of few cycloaromatics is one or two, and the aromatic ring number of the condensed-nuclei aromatics is three or three
More than a.
2. according to the method described in claim 1, wherein, the hydrogenated oil of the condensed-nuclei aromatics oil obtained through hydrogenated processing is at 20 DEG C
Refractive index be 1.52-1.6.
3. according to the method described in claim 1, wherein, the extraction solvent contains main solvent and secondary solvent, with extraction solvent
Gross mass on the basis of, the content of secondary solvent is 0.2-10 weight %, and the content of main solvent is 90-99.8 weight %.
4. according to the method described in claim 3, wherein, on the basis of the gross mass of extraction solvent, the content of secondary solvent is 1-
The content of 8 weight %, main solvent are 92-99 weight %.
5. according to the method described in claim 1,3 or 4, wherein the mass ratio of extraction solvent and feedstock oil is 0.5:1 to 6:1.
6. according to the method described in claim 5, wherein, the mass ratio of extraction solvent and feedstock oil is 1:1 to 4:1.
7. according to the method described in claim 1, wherein, before feedstock oil is contacted with extraction solvent, first by feedstock oil with it is pre-
Solvent mixing is handled, the pre-treatment solvents contain main solvent and secondary solvent, secondary molten on the basis of the gross mass of pre-treatment solvents
The content of agent be more than 0 weight % to less than or be equal to 8 weight %, the content of main solvent is more than or equal to 92 weight % to small
In 100 weight %.
8. according to the method described in claim 7, wherein, on the basis of the gross mass of pre-treatment solvents, the content of secondary solvent is
The content of 1-4 weight %, main solvent are 96-99 weight %.
9. method according to claim 7 or 8, wherein the mass ratio of pre-treatment solvents and feedstock oil is 0.02:1 to
0.5:1。
10. according to the method described in claim 9, wherein, the mass ratio of pre-treatment solvents and feedstock oil is 0.05:1 to 0.3:
1。
11. according to the method described in any one of claim 1,3-4 and 7-8, wherein by feedstock oil or feedstock oil and in advance
The mixture of processing solvent contacts the method for carrying out solvent extraction with extraction solvent：By feedstock oil or feedstock oil and pre- place
The mixture and extraction solvent counter current contacting in extraction tower for managing solvent obtain raffinate from extracting column overhead, and removal solvent obtains
To raffinating oil containing few cycloaromatics, Extract is obtained from extraction tower bottom of tower, removal solvent obtains the extraction containing condensed-nuclei aromatics
Oil, the extracting column overhead temperatures are 45 DEG C to 120 DEG C, and the extraction tower column bottom temperature is 35 DEG C to 95 DEG C.
12. according to the method for claim 11, wherein the extracting column overhead temperatures are 50 DEG C to 90 DEG C, the extracting
Tower column bottom temperature is 40 DEG C to 80 DEG C.
13. according to the method described in any one of claim 1,3-4 and 7-8, wherein the main solvent in the extraction solvent
And the main solvent in pre-treatment solvents is each independently selected from furfural, phenol, dimethyl sulfoxide (DMSO) and N-Methyl pyrrolidone
It is one or more；
The secondary solvent in secondary solvent and pre-treatment solvents in the extraction solvent is each independently selected from water, low-carbon alcohols and low
It is one or more in carbon ketone；The low-carbon alcohols are the one or more of the fatty alcohol that carbon atom number is 1-8, and the low-carbon ketone is
Carbon atom number is the alkenolic one or more of 3-6.
14. according to the method for claim 13, wherein the low-carbon alcohols are selected from ethyl alcohol, isopropanol, normal propyl alcohol, n-butanol
With it is one or more in n-hexyl alcohol, the low-carbon ketone is one or more in butanone, pentanone and hexanone.
15. method according to claim 1 or 2, wherein the tapped oil containing condensed-nuclei aromatics is carried out to the item of hydrotreating
Part includes：Hydrogen partial pressure is 2-24MPa, volume space velocity 0.1-2h-1, hydrogenation temperature is 280-380 DEG C, catalyst be containing Ni and
RCS-31 hydrogenation catalysts of the Mo as active component, and/or make containing Ni, W, Mo the RL-2 hydrogenation catalysts of active component.
16. according to the method for claim 15, wherein hydrogen partial pressure 6-18MPa, volume space velocity 0.5-1.2h-1, add hydrogen
Temperature is 300-350 DEG C.
17. according to the method described in claim 1, wherein, the tapped oil of refinery's lube base oil solvent extraction production
For the lubex and lubricating oil solvent of the second line of distillation of crude oil, the line that subtracts three, the line that subtracts four or frivolous coal tar
The dewaxed oil of refined tapped oil and the second line of distillation of crude oil, the line that subtracts three, the line that subtracts four or frivolous coal tar dewaxed oil solvent essence
It is one or more in tapped oil processed.
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| BR112021015453A2 (en) | 2019-02-05 | 2021-11-23 | Regen Iii Corp | Method and system for refining and improving used oil |
| CN111560266B (en) * | 2019-02-13 | 2022-08-19 | 中国海洋石油集团有限公司 | Aluminum foil rolling oil base oil and preparation method thereof |
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| CN114437760B (en) * | 2020-10-30 | 2023-12-22 | 中石油克拉玛依石化有限责任公司 | Dewaxing method for raw oil |
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