CN106929100A - 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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- CN106929100A CN106929100A CN201511008851.1A CN201511008851A CN106929100A CN 106929100 A CN106929100 A CN 106929100A CN 201511008851 A CN201511008851 A CN 201511008851A CN 106929100 A CN106929100 A CN 106929100A
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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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- Polymers & Plastics (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The present invention relates to oil and petroleum distillate manufacture field, a kind of preparation method of aromatic rubber oil is disclosed, the method includes：Feedstock oil is contacted with extraction solvent, obtain raffinate and Extract, after removal solvent, respectively obtain raffinating oil containing few PAH and the tapped oil containing condensed-nuclei aromatics, the hydrogenated treatment of tapped oil containing condensed-nuclei aromatics obtains the hydrogenated oil of condensed-nuclei aromatics oil, wherein, refractive index of the hydrogenated hydrogenated oil for processing the condensed-nuclei aromatics oil for obtaining at 20 DEG C is 1.5-1.61, the feedstock oil is rich in aromatic naphtha, Part I and Part II should be contained rich in aromatic naphtha, the Part I is the tapped oil and/or catalytic cracking clarified oil of refinery's lube base oil solvent extraction production, the Part II is the hydrogenated oil of the condensed-nuclei aromatics oil, wherein, the aromatic ring number of few PAH is one or two, the aromatic ring number of the condensed-nuclei aromatics is three or more than three.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 method of aromatic rubber oil.
Background technology
It is to improve rubber workability and easily mixing property in process of production, and rubber is elastic and soft
The characteristics such as toughness, generally add rubber oil in the production process of rubber.Rubber oil is by its chemical composition
Difference, is divided into paraffinic, naphthenic type and aromatic hydrocarbon rubber oil.Aromatic rubber oil (Distillate
Aromatic Extract, are abbreviated as DAE) with aromatic carbon content is high, density is big, viscosity is high and polarity
Rubber compatibility is good and be the excellent of butadiene-styrene rubber used by tire and footwear product the features such as superior processing characteristics
Good filler, DAE typically constitutes from 30% or so of rubber gross mass.Due to butadiene-styrene rubber be butadiene and
The random copolymer of styrene, copolymer side chain carries phenyl ring, therefore, aromatic hydrocarbons in butadiene-styrene rubber filling oil
Content is higher, and filling oil is better with the high molecular compatibility of butadiene-styrene rubber, the performance improvement of oil-extended rubber
Better.DAE is usually to be produced through solvent refining unit by feedstock oil in lube base oil production technology
Tapped oil or oil slurry from catalytically cracked heavy oil through reprocessing or blending produce.
From 1 day January in 2010, tire and its accessory into EU market need to be referred to using it is met
(polycyclic aromatic hydrocarbon content that IP346 methods are measured is less than 3%, benzo (a) to make 2005/69/EC quality requirements
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, eight kinds of condensed-nuclei aromatics total contents of benzo (e) anthracene and dibenzo (a, h) anthracene are not more than
Filling oil production 10mg/kg), the U.S. also makes similar production tire and fills in succession with Japan
The quality standard of oil.China's tyre industry is typical export-oriented industry, about 45% tire product outlet
European Union or the U.S., therefore, raising of the above-mentioned country to rubber filling oil quality standard has a strong impact on
The export business of China's tyre industry.
At present, the existing many scientific researches of China or production unit develop the life for meeting European Union environmental protection index request
Produce the tire oily patented technology of filling.CN102453538A discloses a kind of environmentally friendly tyre aromatic oil
Production method, the method with lubex as raw material, after the hydrogenated treatment of feedstock oil,
The hydrotreating oil of raw material produces tire environment-friendly rubber oil through solvent extraction again.Although the method refers to and adopting
Feedstock oil is hydrogenated with suitable catalyst for hydro-upgrading and under conditions of relative mitigation, can be dropped
Low aromatic hydrocarbons loss, but, from the angle that aromatic rubber oil control of product quality and resource make full use of
Say, the production method of the aromatic naphtha of prior art still has larger room for improvement.
The content of the invention
The purpose of the present invention be overcome in the prior art aromatic rubber oil control of product quality difference and can not
Make full use of the defect of petroleum resources and providing one kind can improve environment-friendly type aromatic rubber oil yield and matter
Amount, and the aromatic rubber oil preparation method of petroleum resources can be made full use of.
To achieve these goals, the present invention provides a kind of preparation method of aromatic rubber oil, the method bag
Include：Feedstock oil is contacted with extraction solvent, raffinate and Extract is obtained, after removal solvent, respectively
To raffinating oil containing few PAH and the tapped oil containing condensed-nuclei aromatics, the tapped oil containing condensed-nuclei aromatics
Hydrogenated treatment obtains the hydrogenated oil of condensed-nuclei aromatics oil, wherein, it is hydrogenated to process the condensed-nuclei aromatics oil for obtaining
Refractive index of the hydrogenated oil at 20 DEG C be 1.5-1.61, the feedstock oil is that, rich in aromatic naphtha, this is rich in
Aromatic naphtha contains Part I and Part II, and the Part I is taken out for refinery's lube base oil solvent
The tapped oil and/or catalytic cracking clarified oil of production are put forward, the Part II is adding for the condensed-nuclei aromatics oil
Hydrogen oil, wherein, the aromatic ring number of few PAH is one or two, the aromatic ring of the condensed-nuclei aromatics
Number is three or more than three.
CN102453538A discloses a kind of production method of environmentally friendly tyre aromatic oil, the method bag
Include feedstock oil (furfural extract oil) hydrogenation, and the hydrogenated oil of feedstock oil is prepared into environmental protection through solvent extraction
Type aromatic hydrocarbon rubber extender oil.Although the method refers to that feedstock oil hydroconversion condition relaxes, and can reduce aromatic hydrocarbons damage
Lose, but do not propose influence of the hydrogenation reaction degree of feedstock oil to end product quality, and the method
The tapped oil (condensed-nuclei aromatics oil) of the hydrotreating oil solvent extracting still containing the single double ring arene in part is straight
Discharger is connect, is unfavorable for making full use of for petroleum resources.
The present invention is split using the tapped oil containing refinery's lube base oil solvent extraction production and/or catalysis
The condensed-nuclei aromatics obtained after the Extract removal solvent for changing solvent extraction production in clarified oil, and the present invention
The mixture of the hydrogenated oil of oil makees feedstock oil, and feedstock oil obtains the raffinate containing few PAH through solvent extraction
Oil makees environment-friendly type aromatic hydrocarbon rubber extender oil, and the tapped oil containing condensed-nuclei aromatics makees the raw material of hydrogenation plant, and
The refractive index of the hydrogenated oil after by controlling the tapped oil containing condensed-nuclei aromatics hydrogenated, can most preferably limit ground
More than the ring of environmental-friendly rubber filling oil undesirable components three in the tapped oil containing condensed-nuclei aromatics and three rings
Aromatic hydrogenation saturation is converted into the oily ideal composition of the filling such as monocyclic or double ring arene, and then effectively improves environmental protection
The quality (CA values) and yield of type rubber filling oil.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Brief description of the drawings
Accompanying drawing is, for providing a further understanding of the present invention, and to constitute the part of specification, with
Following specific embodiment is used to explain the present invention together, but is not construed as limiting the invention.
In accompanying drawing：
Fig. 1 is a kind of schematic flow diagram of the preparation of the aromatic rubber oil of preferred embodiment of the invention.
Description of reference numerals
1 raw material oil pipeline；2 first static mixers；3 feedstock oils are detected and control device；
4 pre-treatment solvents pipelines；5 mixed 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 means；
13 hydrogenated oil pipeloops.
Specific embodiment
Specific embodiment of the invention is described in detail below.It should be appreciated that this place is retouched
The specific embodiment stated is merely to illustrate and explain the present invention, and is not intended to limit the invention.
According to the present invention, the preparation method of the aromatic rubber oil includes：Feedstock oil is connect with extraction solvent
Touch, obtain raffinate and Extract, after removal solvent, respectively obtain containing few PAH raffinating oil with
Tapped oil containing condensed-nuclei aromatics, the hydrogenated treatment of the tapped oil containing condensed-nuclei aromatics obtains condensed-nuclei aromatics oil
Hydrogenated oil, wherein, hydrogenated refractive index of the hydrogenated oil at 20 DEG C for processing the condensed-nuclei aromatics oil for obtaining
It is 1.5-1.61, the feedstock oil is that, rich in aromatic naphtha, should contain Part I and second rich in aromatic naphtha
Part, the Part I is that the tapped oil of refinery's lube base oil solvent extraction production and/or catalysis are split
Change clarified oil, the Part II is the hydrogenated oil of the condensed-nuclei aromatics oil, wherein, few PAH
Aromatic ring number be one or two, the aromatic ring number of the condensed-nuclei aromatics is three or more than three.
Tapped oil that feedstock oil is produced through solvent extraction (condensed-nuclei aromatics oil) for mainly containing three rings and three rings with
Material based on upper aromatic hydrocarbons, is the undesirable components of environmentally-frierubber rubber filling oil, and feedstock oil is through solvent extraction
Production raffinate oil (environment-friendly type aromatic rubber oil) be mainly contain it is monocyclic and bicyclic based on material,
It is 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,
Aromatic hydrogenations more than three rings and three rings can be converted into environmentally-frierubber rubber filling oil ideal composition Dan Shuan
PAH, it is possible to prevent excessive hydrogenation saturation to be converted into cycloalkane, and cause the reduction of product aromatic carbon content.
The present inventor it has furthermore been found that content of the refractive index not with oil product aromatic hydrocarbons is directly related,
But have certain incidence relation with the carbon type of hydrocarbon in oil product.Inventor's discovery, aromatic carbon content (CA%)
Higher, the refractive index of the hydrogenated oil of condensed-nuclei aromatics oil is higher；Cycloalkanes carbon content (CN%) and alkane carbon
Content (CP%) is higher, and the refractive index of the hydrogenated oil of condensed-nuclei aromatics oil is lower.Therefore, by control
The hydrogenation reaction degree of the tapped oil containing condensed-nuclei aromatics, the refractive index of the hydrogenated oil after making its hydrogenated exists
In the scope of the present invention, namely refractive index is 1.5-1.61, can both realize three rings and three ring above aromatic hydrocarbons
Hydrogenation saturation is single double ring arene, can avoid causing product aromatic carbon content because of excessive hydrogenation saturated reaction again
The problem of reduction.
Further preferably, control hydrogenation degree causes the hydrogenated oil of the hydrogenated condensed-nuclei aromatics oil for processing and obtaining
Refractive index at 20 DEG C can be better achieved goal of the invention of the invention for 1.52-1.6.
According to the present invention, the tapped oil obtained after being separated through solvent extraction and through solvent (condensed-nuclei aromatics oil)
The hydrogenated oil of the condensed-nuclei aromatics oil by being obtained after hydrotreating can be directly as the second of feedstock oil
Divide charging carries out solvent extraction step together with Part I charging.Therefore, Part I and Part II
Refining ratio of mixing be not particularly limited, appropriate Part I can be selected according to the disposal ability of equipment
With the inlet amount of Part II.
According to the present invention, the feedstock oil is the Part II that should contain rich in aromatic naphtha rich in aromatic naphtha
Come from feedstock oil is obtained after the Extract after solvent extraction removes solvent extraction in this method
The hydrogenated treatment of oil obtains the hydrogenated oil of condensed-nuclei aromatics oil.Using the hydrogenated oil of condensed-nuclei aromatics oil as being rich in
Aromatic naphtha loops back solvent extraction system as feedstock oil, can be by condensed-nuclei aromatics oil by gained after hydrogenation
Monocyclic, double ring arene in hydrogenation products are separated again by solvent extraction process, and as mesh
Mark product environment-friendly aromatic rubber oil, and then the yield and aromatic carbon content of environment-friendly type aromatic rubber oil are improve,
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 returned by the condensed-nuclei aromatics hydrogenated oil that hydrogenation is obtained making
It is the charging of solvent extraction system, you can to realize improving the yield and aromatic carbon of environment-friendly type aromatic rubber oil
The purpose of content.Under preferable case, the hydrogenated oil of whole condensed-nuclei aromatics oil is returned as solvent extraction system
The filling oil such as one of charging of system, the monocyclic, double ring arene being beneficial in condensed-nuclei aromatics oil hydrogenated oil are preferable
Component is entered into final environment-friendly rubber oil product component.
According to the present invention, the extraction solvent usually contains main solvent and secondary solvent, with the total of extraction solvent
On the basis of quality, the content of secondary solvent can be 0.2-10 weight %, and the content of main solvent can be
90-99.8 weight %, it is preferable that the content of secondary solvent is 1-8 weight %, and the content of main solvent is 92-99
Weight %.
According to the present invention, extraction solvent can be 0.5 with the mass ratio of the hydrogenated oil of feedstock oil:1 to 6:1,
Preferably 1:1 to 4:1.Controlled in aforementioned proportion scope by by the mass ratio of feedstock oil and extraction solvent
It is interior, three rings and three ring above aromatic hydrocarbons and single double ring arene and alkane in the feedstock oil can be better achieved
Be sufficiently separated.
According to the present invention, the extraction solvent usually contains main solvent and secondary solvent, wherein, main solvent can
Think the conventional main solvent in this area.Under preferable case, the main solvent is selected from furfural, phenol, diformazan
One or more in base sulfoxide and 1-METHYLPYRROLIDONE.The secondary solvent can be this area routine
Secondary solvent.Under preferable case, the secondary solvent is selected from the one kind or many in water, low-carbon alcohols and low-carbon (LC) ketone
Kind；The low-carbon alcohols are one or more of the fatty alcohol that carbon number is 1-8, further preferably, institute
State one or more during low-carbon alcohols are selected from ethanol, isopropanol, normal propyl alcohol, n-butanol and n-hexyl alcohol；Institute
It is alkenolic one or more of 3-6, further preferably, the low-carbon (LC) for carbon number to state low-carbon (LC) ketone
Ketone is selected from one or more in butanone, pentanone and hexanone.
According to the present invention, under preferable case, before feedstock oil is contacted with extraction solvent, the method is also
Including feedstock oil is mixed with pre-treatment solvents, to realize reducing the purpose of feedstock oil viscosity.The pre- place
Reason solvent usually contains main solvent and secondary solvent, on the basis of the gross mass of pre-treatment solvents, secondary solvent
Content is that the content of main solvent is more than or equal to 92 to less than or equal to 8 weight % more than 0 weight %
To 100 weight % are less than, further preferably, the content of secondary solvent is 1-4 weight % to weight %, and master is molten
The content of agent is 96-99 weight %.
According to the present invention, the feedstock oil can be with known in the art various with the mixing of pre-treatment solvents
Carried out in mixing apparatus, for example, can be carried out in static mixer, can also be dynamic with agitating paddle
Carried out in state blender.
According to the present invention, the pre-treatment solvents can be 0.02 with the mass ratio of feedstock oil:1 to 0.5:1,
Preferably 0.05:1 to 0.3:1.Mix in the range of aforementioned proportion with pre-treatment solvents by by feedstock oil,
Three rings in the feedstock oil and three ring above aromatic hydrocarbons and single double ring arene and alkane can be better achieved
Be sufficiently separated.
The species selection of main solvent in the pre-treatment solvents and secondary solvent generally respectively with extraction solvent
In main solvent it is identical with the species selection of secondary solvent, it is further preferred that main solvent and pair in pre-treatment solvents
Solvent is identical with the main solvent in extraction solvent and secondary solvent respectively.
According to the present invention, feedstock oil or feedstock oil are connect with the mixture of pre-treatment solvents with extraction solvent
Touching carries out solvent extraction and is carried out in extraction tower.The method includes：By feedstock oil or feedstock oil and pre- place
The mixture and extraction solvent for managing solvent are fully contacted in extraction tower, and raffinate is obtained by extracting column overhead,
Separated by solvent, raffinate oil (aromatic rubber oil) is isolated from raffinate, obtained from extraction tower bottom of towe
To Extract, separated by solvent, tapped oil (condensed-nuclei aromatics oil) is isolated from Extract.It is described
Extracting column overhead temperatures can be 45 DEG C to 120 DEG C, preferably 50 DEG C to 90 DEG C, the extraction tower tower
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 the condition that the tapped oil containing condensed-nuclei aromatics carries out hydrotreating is ensured into warp
The refractive index of the hydrogenated oil of the condensed-nuclei aromatics oil obtained after hydrogenation is 1.5-1.61, under preferable case, through adding
The refractive index of the hydrogenated oil of the condensed-nuclei aromatics oil obtained after hydrogen is 1.52-1.6.
It is described generally to wrap the condition that the tapped oil containing condensed-nuclei aromatics carries out hydrotreating according to the present invention
Hydrogen dividing potential drop, air speed and hydrogenation temperature are included, under preferable case, hydrogen dividing potential drop is 2-24MPa, and air speed is 0.1-2h-1,
Hydrogenation temperature is 280-380 DEG C, and further preferably, hydrogen dividing potential drop is 6-18MPa, and air speed is 0.5-1.2h-1,
Hydrogenation temperature is 300-350 DEG C.
According to the present invention, the tapped oil containing condensed-nuclei aromatics is hydrogenated with into used hydrogenation catalyst is
Various Hydrobon catalysts known in the field, the hydrogenation catalyst includes carrier and is supported on this
Active component on carrier.The carrier can be the various carriers in existing Hydrobon catalyst, example
Such as, can be selected from one or more in amorphous silicon aluminum oxide.The activearm of the hydrogenation catalyst
Divide one or more can be selected from Mo, Ni, Co and W, preferably Ni and/or Mo is optimal
Choosing, the hydrogenation catalyst be containing Ni and Mo as active component RCS-31 hydrogenation catalysts and
/ or make the RL-2 hydrogenation catalysts of active component containing Ni, W, Mo.The system of the hydrogenation catalyst
The standby preparation side that may be referred to well known to a person skilled in the art Hydrobon catalyst of the prior art
Method, can also be commercially available, for example, described add containing Ni and Mo as the RCS-31 of active component
Hydrogen catalyst and can be with commercially available containing the RL-2 hydrogenation catalysts that Ni, W, Mo make active component
From Sinopec catalyst branch company.
In the present invention, the feedstock oil is the Part I that should contain rich in aromatic naphtha rich in aromatic naphtha,
The tapped oil of refinery lube base oil solvent extraction production refers to the second line of distillation of crude oil, the line that subtracts three, subtracts
The lubex and lubex of four lines or frivolous coal tar
The solvent essence of the dewaxed oil of the second line of distillation of dewaxed oil and crude oil, the line that subtracts three, the line that subtracts four or frivolous coal tar
One or more in tapped oil processed.
Below in conjunction with accompanying drawing 1, a kind of preparation of the aromatic rubber oil of preferred embodiment of the invention is illustrated.
From raw material oil pipeline 1 rich in aromatic naphtha：What refinery's lube base oil solvent extraction was produced takes out
Fuel-displaced and/or catalytic cracking clarified oil is managed with the hydrogenated oil of the condensed-nuclei aromatics oil from hydrogenation oil pipeline 13
After mixing in line, it is sufficiently mixed that (feedstock oil is detected and control device 3 is available through the first static mixer 2
In two kinds of flows of charging of regulation and control), then mixed through with the pre-treatment solvents from pre-treatment solvents pipeline 4
After closing the mixing of feed line 5, it is well mixed through the second static mixer 6, through extraction device raw material oil pipe
Line 7 enter solvent extraction apparatus 8, with extraction solvent in solvent extraction apparatus 8 counter current contacting, raffinate
After liquid is through solvent recovery removal solvent, through the discharger of tubulature line 9 of raffinating oil out, aromatic rubber oil is obtained,
Extract obtains tapped oil (condensed-nuclei aromatics oil) after solvent recovery removal solvent, and condensed-nuclei aromatics oil is through adding
Hydrogen production device raw material oil pipeline 10 enters hydrogenation plant 11, the hydrogenated oil detection of hydrogenated oil of condensed-nuclei aromatics oil
After device 12 is detected, then hydrogenated oil circulating pipe line 13 returns to feedstock oil.Accompanying drawing does not indicate raffinate
Liquid and Extract solvent recovering system.
The preferred embodiment of the present invention described in detail above, but, the present invention is not limited to above-mentioned reality
The detail in mode is applied, in range of the technology design of the invention, can be to technical side of the invention
Case carries out various simple variants, and these simple variants belong to protection scope of the present invention.
It is further to note that each particular technique feature described in above-mentioned specific embodiment,
In the case of reconcilable, can be combined by any suitable means, in order to avoid unnecessary
Repeat, the present invention is no longer separately illustrated to various possible combinations.
Additionally, can also be combined between a variety of implementation methods of the invention, as long as its
Without prejudice to thought of the invention, it should equally be considered as content disclosed in this invention.
Below will the present invention will be described in detail by embodiment.
In following examples, hydrogenated oil refractive index is measured by SH/T0724 methods, environment-friendly type aromatic hydrocarbons rubber
The aromatic carbon content of glue oil is measured by ASTM D2140 methods, the polycyclic aromatic hydrocarbon of environment-friendly type aromatic rubber oil
Content is measured by the methods of NB/SH/T 0838, benzo (a) the pyrene content and benzene of environment-friendly type aromatic rubber oil
And eight kinds of condensed-nuclei aromatics total contents such as (a) pyrene are measured by the methods of SN/T 1877.3.
The computing formula of environment-friendly type aromatic rubber oil (raffinating oil) yield：Yield %=(take out by solvent extraction
Excess oil × 100)/solvent extraction feedstock oil (Part I containing feedstock oil and feedstock oil Part II).
Embodiment 1
The present embodiment is used for the preparation of the aromatic rubber oil for illustrating present invention offer.
Part I is the solvent refining tapped oil of crude oil second line of distillation dewaxed oil in feedstock oil, and its property is shown in Table
1。
The tapped oil of Part I second line of distillation dewaxed oil is oily with Part II condensed-nuclei aromatics in feedstock oil adds
After hydrogen oil mixing, then mix with pre-treatment solvents, and in extraction tower with extraction solvent counter current contacting, in advance
The main solvent for the treatment of solvent and extraction solvent is 1-METHYLPYRROLIDONE, and secondary solvent is isopropanol,
Secondary solvent is the 3% of respective solvent gross weight, and the content of main solvent is respective solvent gross weight
97%.Pre-treatment solvents are 0.1 with the mass ratio of feedstock oil:1, the quality of extraction solvent and feedstock oil
Than being 3.5:1, extracting column overhead and column bottom temperature are respectively 80 DEG C and 50 DEG C.Taken out from the tower top of extraction tower
Raffinate oil (environment-friendly type aromatic rubber oil) is isolated in extraction raffinate, is separated from the Extract of extraction tower bottom of towe
Go out tapped oil (condensed-nuclei aromatics oil), raffinate oil yield and property are shown in Table 2.
The tapped oil (condensed-nuclei aromatics oil) obtained after being separated through solvent by bottom of towe after above-mentioned solvent extraction is entered
Row hydrotreating, hydrotreating catalyst is that the RL-2 hydrogenation of Sinopec catalyst branch company production is urged
Agent, hydrogen dividing potential drop 12MPa, volume space velocity 1.2h-1, 315 DEG C of hydrogenation plant feedstock inlet temperature is thick
The refractive index of the hydrogenated oil of cyclophane hydrocarbon ils is shown in Table 2, and the hydrogenated oil of gained condensed-nuclei aromatics oil is used as feedstock oil
Part II feeds.
Comparative example 1
This comparative example is used for the preparation of the aromatic rubber oil for illustrating reference method.
Using feedstock oil same as Example 1, identical hydrotreating catalyst, and identical is molten
Agent composition and solvent extraction condition, unlike, hydrogen dividing potential drop 17MPa, volume space velocity 0.5h-1, hydrogenation
355 DEG C of device feedstock inlet temperature, 20 DEG C of refractive indexes of the hydrogenated oil of the condensed-nuclei aromatics oil for controlling to obtain are
1.4915.The condensed-nuclei aromatics oil 20 DEG C of refractive indexes of hydrogenated oil, raffinate oil (environment-friendly type aromatic rubber oil)
Property is shown in Table 2.
Comparative example 2
This comparative example is used for the preparation of the aromatic rubber oil for illustrating reference method.
Using feedstock oil same as Example 1, identical hydrotreating catalyst, and identical is molten
Agent composition and solvent extraction condition, unlike, hydrogen dividing potential drop 2MPa, volume space velocity 2.5h-1, hydrogenation dress
270 DEG C of feedstock inlet temperature is put, 20 DEG C of refractive indexes for controlling the hydrogenated oil of the condensed-nuclei aromatics for obtaining oil are
1.6217.20 DEG C of refractive indexes of hydrogenated oil, (environment-friendly type aromatic rubber oil) property of raffinating oil of condensed-nuclei aromatics oil
Matter is shown in Table 2.
Embodiment 2
The present embodiment is used for the preparation of the aromatic rubber oil for illustrating present invention offer.
Part I is the dewaxed oil of the crude oil line tapped oil that subtracts three in feedstock oil, and its property is shown in Table 1.
In feedstock oil the dewaxed oil of the Part I line tapped oil that subtracts three and Part II condensed-nuclei aromatics oil plus
After hydrogen oil mixing, then mix with pre-treatment solvents, and in extraction tower with extraction solvent counter current contacting, in advance
The main solvent for the treatment of solvent and extraction solvent is phenol, and secondary solvent is pentanone, and secondary solvent is
The 2% of respective solvent gross weight, the content of main solvent is the 98% of respective solvent gross weight.Pretreatment
Solvent is 0.3 with the mass ratio of feedstock oil:1, extraction solvent is 5 with the mass ratio of feedstock oil:1, extraction tower
Tower top and column bottom temperature are respectively 95 DEG C and 80 DEG C.Raffinate is isolated from the tower top raffinate of extraction tower
Oily (environment-friendly type aromatic rubber oil), isolates tapped oil (condensed ring virtue from the Extract of extraction tower bottom of towe
Hydrocarbon ils), raffinate oil yield and property are shown in Table 2.
The tapped oil (condensed-nuclei aromatics oil) obtained after being separated through solvent by bottom of towe after above-mentioned solvent extraction is entered
Row hydrotreating, hydrotreating catalyst is that the RL-2 hydrogenation of Sinopec catalyst branch company production is urged
Agent, hydrogen dividing potential drop 6MPa, volume space velocity 0.5h-1, 340 DEG C of hydrogenation plant feedstock inlet temperature, condensed ring
The refractive index of the hydrogenated oil of aromatic naphtha is shown in Table 2, and the hydrogenated oil of gained condensed-nuclei aromatics oil is used as the of feedstock oil
Two parts feed.
Embodiment 3
The present embodiment is used for the preparation of the aromatic rubber oil for illustrating present invention offer.
Part I is the tapped oil of the crude oil line that subtracts four in feedstock oil, and its property is shown in Table 1.
The Part I line tapped oil that subtracts four mixes with the hydrogenated oil of Part II condensed-nuclei aromatics oil in feedstock oil
Afterwards, then with pre-treatment solvents mix, and in extraction tower with extraction solvent counter current contacting, pre-treatment solvents
Furfural is with the main solvent of extraction solvent, secondary solvent is water, and it is total that secondary solvent is respective solvent
The 1% of weight, the content of main solvent is the 99% of respective solvent gross weight.Pre-treatment solvents and raw material
The mass ratio of oil is 0.5:1, extraction solvent is 1.5 with the mass ratio of feedstock oil:1, extract column overhead and tower
Bottom temperature is respectively 70 DEG C and 60 DEG C.(environmental protection of raffinating oil is isolated from the tower top raffinate of extraction tower
Type aromatic rubber oil), tapped oil (condensed-nuclei aromatics oil) is isolated from the Extract of extraction tower bottom of towe, take out
Excess oil yield and property are shown in Table 2.
The tapped oil (condensed-nuclei aromatics oil) obtained after being separated through solvent by bottom of towe after above-mentioned solvent extraction is entered
Row hydrotreating, hydrotreating catalyst is that the RL-2 hydrogenation of Sinopec catalyst branch company production is urged
Agent, hydrogen dividing potential drop 8MPa, volume space velocity 0.8h-1, 320 DEG C of hydrogenation plant feedstock inlet temperature, condensed ring
The refractive index of the hydrogenated oil of aromatic naphtha is shown in Table 2, and the hydrogenated oil of gained condensed-nuclei aromatics oil is used as the of feedstock oil
Two parts feed.
Embodiment 4
The present embodiment is used for the preparation of the aromatic rubber oil for illustrating present invention offer.
Part I is the dewaxed oil of the frivolous coal tar tapped oil of crude oil in feedstock oil, and its property is shown in Table 1.
The dewaxed oil of the frivolous coal tar tapped oil of Part I and Part II condensed-nuclei aromatics oil in feedstock oil
Hydrogenated oil mixing after, then mix with pre-treatment solvents, and in extraction tower with extraction solvent counter current contacting,
The main solvent of pre-treatment solvents and extraction solvent is dimethyl sulfoxide (DMSO), and secondary solvent is n-hexyl alcohol, secondary molten
Agent content is the 8% of respective solvent gross weight, and the content of main solvent is respective solvent gross weight
92%.Pre-treatment solvents are 0.2 with the mass ratio of feedstock oil:1, extraction solvent is with the mass ratio of feedstock oil
2.5:1, extracting column overhead and column bottom temperature are respectively 120 DEG C and 90 DEG C.From the tower top raffinate of extraction tower
In isolate raffinate oil (environment-friendly type aromatic rubber oil), isolated from the Extract of extraction tower bottom of towe and taken out
Fuel-displaced (condensed-nuclei aromatics oil), raffinate oil yield and property are shown in Table 2.
The tapped oil (condensed-nuclei aromatics oil) obtained after being separated through solvent by bottom of towe after above-mentioned solvent extraction is entered
Row hydrotreating, hydrotreating catalyst is the RCS-31 hydrogenation of Sinopec catalyst branch company production
Catalyst, hydrogen dividing potential drop 18MPa, volume space velocity 1.5h-1, 350 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, and the hydrogenated oil of gained condensed-nuclei aromatics oil is used as feedstock oil
Part II charging.
Embodiment 5
The present embodiment is used for the preparation of the aromatic rubber oil for illustrating present invention offer.
Part I is catalytic cracking clarified oil in feedstock oil, and its property is shown in Table 1.
Part I catalytic cracking clarified oil is mixed with the hydrogenated oil of Part II condensed-nuclei aromatics oil in feedstock oil
After conjunction, then mix with pre-treatment solvents, and in extraction tower with extraction solvent counter current contacting, pre-process it is molten
The main solvent of agent and extraction solvent is furfural, and secondary solvent is ethanol, and secondary solvent is each self-dissolving
The 5% of agent gross weight, the content of main solvent is the 95% of respective solvent gross weight.Pre-treatment solvents with
The mass ratio of feedstock oil is 0.4:1, extraction solvent is 5 with the mass ratio of feedstock oil:1, extracting column overhead and
Column bottom temperature is respectively 75 DEG C and 70 DEG C.(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) is isolated from the Extract of extraction tower bottom of towe,
Raffinate oil yield and property are shown in Table 2.
The tapped oil (condensed-nuclei aromatics oil) obtained after being separated through solvent by bottom of towe after above-mentioned solvent extraction is entered
Row hydrotreating, hydrotreating catalyst is the RCS-31 hydrogenation of Sinopec catalyst branch company production
Catalyst, hydrogen dividing potential drop 20MPa, volume space velocity 2.0h-1, 370 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, and the hydrogenated oil of gained condensed-nuclei aromatics oil is used as feedstock oil
Part II charging.
Embodiment 6
The present embodiment is used for the preparation of the aromatic rubber oil for illustrating present invention offer.
Part I is the solvent essence of crude oil second line of distillation dewaxed oil in using feedstock oil same as Example 1
Tapped oil processed, identical hydrotreating catalyst and hydroconversion condition, and identical solvent composition and solvent
Extraction conditions, the difference is that, contacted with extraction solvent before carrying out solvent extraction by feedstock oil, will not
Feedstock oil mixes with pre-treatment solvents, and directly feedstock oil is contacted with extraction solvent.The condensed ring virtue for obtaining
20 DEG C of refractive indexes of the hydrogenated oil of hydrocarbon ils, the yield and property of (environment-friendly type aromatic rubber oil) of raffinating oil are shown in
Table 2.
Embodiment 7
The present embodiment is used for the preparation of the aromatic rubber oil for illustrating present invention offer.
Part I is the solvent essence of crude oil second line of distillation dewaxed oil in using feedstock oil same as Example 1
Tapped oil processed, identical hydrotreating catalyst and hydroconversion condition, and identical solvent extraction condition,
Unlike, without secondary solvent in extraction solvent and pre-treatment solvents.Obtain condensed-nuclei aromatics oil plus
20 DEG C of refractive indexes of hydrogen oil, the yield and property of (environment-friendly type aromatic rubber oil) of raffinating oil are shown in Table 2.
Embodiment 8
The present embodiment is used for the preparation of the aromatic rubber oil for illustrating present invention offer.
The tapped oil of the line that subtracts four for crude oil of Part I in feedstock oil same as Example 3 is used, it is identical
Hydrotreating catalyst, identical solvent extraction condition, unlike, the hydrogen of hydrotreater point
It is 2MPa to press, volume space velocity 1.2h-1, 280 DEG C of hydrogenation plant feedstock inlet temperature.The condensed ring virtue for obtaining
20 DEG C of refractive indexes of the hydrogenated oil of hydrocarbon ils, the yield and property of (environment-friendly type aromatic rubber oil) of raffinating oil are shown in
Table 2.
Table 1
Table 2
* the computing formula of environment-friendly type aromatic rubber oil (raffinating oil) yield：Yield %=(solvent extraction raffinate oil × 100)
/ solvent extraction feedstock oil (Part I containing feedstock oil and feedstock oil Part II).
Continued 2
* the computing formula of environment-friendly type aromatic rubber oil (raffinating oil) yield：Yield %=(solvent extraction raffinate oil × 100)
/ solvent extraction feedstock oil (Part I containing feedstock oil and feedstock oil Part II).
By 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 yield and aromatic carbon content understand, if the hydrogenated device of condensed-nuclei aromatics oil produces the refraction of hydrogenated oil
Rate exceed scope of the presently claimed invention, although environment-friendly type aromatic rubber oil yield (comparative example 1) or
Environment-friendly type aromatic rubber oil aromatic carbon content (comparative example 2) is slightly higher, but environment-friendly type aromatic rubber oil is corresponding
Aromatic carbon content or yield reduction, that is, comparative example 1 and 2 cannot take into account environment-friendly type aromatic rubber oil yield
It is excellent with aromatic carbon content, and can then be taken into account well using the method for the present invention both has ring higher
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
Result shows, during feedstock oil is through solvent extraction method production environment-friendly type aromatic rubber oil, extraction solvent
Environment-friendly type aromatic rubber can be further improved containing pre-treatment solvents are added in secondary solvent or extracting raw material
The yield and its aromatic carbon content of oil.
Embodiment 3 shows with the environment-friendly type aromatic rubber oil yield of embodiment 8 and the result of aromatic carbon content,
Refractive index of the hydrogenated hydrogenated oil for processing the condensed-nuclei aromatics oil for obtaining of control at 20 DEG C is excellent in the present invention
In the range of choosing, in the case where environment-friendly type aromatic rubber oil aromatic carbon content is suitable, it is possible to increase environment-friendly type virtue
The yield of hydrocarbon rubbers oil.
Embodiment 2-5 further proves adding rich in aromatic naphtha and condensed-nuclei aromatics oil for refinery's secondary operation production
The mixture of hydrogen oil can be produced through the method and meet environmentally friendly index request in European Union 2005/69/EC instructions
Environment-friendly type aromatic rubber oil product.
Claims (10)
1. a kind of preparation method of aromatic rubber oil, the method includes：Feedstock oil is connect with extraction solvent
Touch, obtain raffinate and Extract, after removal solvent, respectively obtain containing few PAH raffinating oil with
Tapped oil containing condensed-nuclei aromatics, the hydrogenated treatment of the tapped oil containing condensed-nuclei aromatics obtains condensed-nuclei aromatics oil
Hydrogenated oil, it is characterised in that
Refractive index of the hydrogenated hydrogenated oil for processing the condensed-nuclei aromatics oil for obtaining at 20 DEG C is 1.5-1.61,
The feedstock oil is that, rich in aromatic naphtha, should contain Part I and Part II rich in aromatic naphtha, described the
A part is the tapped oil and/or catalytic cracking clarified oil of refinery's lube base oil solvent extraction production, institute
The hydrogenated oil that Part II is the condensed-nuclei aromatics oil is stated,
Wherein, the aromatic ring number of few PAH is one or two, and the aromatic ring of the condensed-nuclei aromatics is individual
Number is three or more than three.
2. method according to claim 1, wherein, it is hydrogenated to process the condensed-nuclei aromatics oil for obtaining
Refractive index of the hydrogenated oil at 20 DEG C be 1.52-1.6.
3. method according to claim 1, wherein, the extraction solvent contains main solvent and pair
Solvent, on the basis of the gross mass of extraction solvent, the content of secondary solvent is 0.2-10 weight %, main solvent
Content be 90-99.8 weight %, it is preferable that the content of secondary solvent be 1-8 weight %, the content of main solvent
It is 92-99 weight %.
4. the method according to claim 1 or 3, wherein, the quality of extraction solvent and feedstock oil
Than being 0.5:1 to 6:1, preferably 1:1 to 4:1.
5. method according to claim 1, wherein, before feedstock oil is contacted with extraction solvent,
First feedstock oil is mixed with pre-treatment solvents, the pre-treatment solvents contain main solvent and secondary solvent, with pre-
Process on the basis of the gross mass of solvent, the content of secondary solvent is to less than or equal to 8 weights more than 0 weight %
Amount %, the content of main solvent is to less than 100 weight % more than or equal to 92 weight %, it is preferable that secondary molten
The content of agent is 1-4 weight %, and the content of main solvent is 96-99 weight %.
6. method according to claim 5, wherein, the mass ratio of pre-treatment solvents and feedstock oil
It is 0.02:1 to 0.5:1, preferably 0.05:1 to 0.3:1.
7. the method according to claim 1,3 or 5, wherein, by feedstock oil or feedstock oil with
The mixture of pre-treatment solvents contacts with extraction solvent and carries out the method for solvent extraction and include：By feedstock oil or
The mixture of person's feedstock oil and pre-treatment solvents and extraction solvent counter current contacting in extraction tower, from extraction tower
Tower top obtains raffinate, and removal solvent obtains raffinating oil containing few PAH, obtained from extraction tower bottom of towe
Extract, removal solvent obtains the tapped oil containing condensed-nuclei aromatics, and the extracting column overhead temperatures are 45 DEG C
To 120 DEG C, preferably 50 DEG C to 90 DEG C, the extraction tower column bottom temperature is 35 DEG C to 95 DEG C, preferably
It is 40 DEG C to 80 DEG C.
8. the method according to claim 1,3 or 5, wherein, the master in the extraction solvent is molten
Main solvent in agent and pre-treatment solvents be each independently selected from furfural, phenol, dimethyl sulfoxide (DMSO) and
One or more in 1-METHYLPYRROLIDONE；
The secondary solvent in secondary solvent and pre-treatment solvents in the extraction solvent is each independently selected from
One or more in water, low-carbon alcohols and low-carbon (LC) ketone；The low-carbon alcohols are that carbon number is the fat of 1-8
One or more of alcohol, it is preferable that the low-carbon alcohols be selected from ethanol, isopropanol, normal propyl alcohol, n-butanol and
One or more in n-hexyl alcohol；The low-carbon (LC) ketone is that carbon number is alkenolic one kind or many of 3-6
Kind, it is preferable that the low-carbon (LC) ketone is selected from one or more in butanone, pentanone and hexanone.
9. method according to claim 1 and 2, wherein, by the tapped oil containing condensed-nuclei aromatics
The condition for carrying out hydrotreating includes：Hydrogen dividing potential drop is 2-24MPa, and air speed is 0.1-2h-1, hydrogenation temperature
It it is 280-380 DEG C, it is preferable that hydrogen dividing potential drop is 6-18MPa, air speed is 0.5-1.2h-1, hydrogenation temperature is
300-350℃；Catalyst is the RCS-31 hydrogenation catalysts as active component containing Ni and Mo,
And/or make the RL-2 hydrogenation catalysts of active component containing Ni, W, Mo.
10. method according to claim 1, wherein, refinery's lube base oil solvent is taken out
It is the lubrication oil soluble of the second line of distillation of crude oil, the line that subtracts three, the line that subtracts four or frivolous coal tar to put forward the tapped oil of production
The second line of distillation of the dewaxed oil and crude oil of the refined tapped oil of agent and lubex, subtract three
One or more in the solvent refining tapped oil of the dewaxed oil of line, the line that subtracts four or frivolous coal tar.
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| CN114437760A (en) * | 2020-10-30 | 2022-05-06 | 中石油克拉玛依石化有限责任公司 | Raw oil dewaxing method |
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