KR101651413B1 - Rubber compounding oil, aromatic compound-containing base oil, and methods for producing same - Google Patents

Abstract

The present invention relates to a thermosetting resin composition comprising 50 mass% or more of a total aromatic content according to ASTM D 2007 or ASTM D 2549, a flash point of 250 ° C or more, a difference between a pour point and a glass transition point of 45 ° C or more, And the total content of the specific aromatic compounds in the following 1) to 8) is 10 mass ppm or less. 1) Benzo (a) Pyrene (BaP) 2) Benzo (e) Pyrene 3) Benzo a) Anthracene (BaA) 4) Chrysene (CHR) 5) ) Benzo (j) fluoransen (BjFA) 7) benzo (k) fluoransen (BkFA) 8) dibenzo (a, h) anthracene (DBAhA)

Description

Rubber compounding oils and aromatic-containing base oils, and methods for their production {Rubber compounding oils, aromatic compound-containing base oils, and methods for producing same)

The present invention relates to a rubber compounded oil and an aromatic-containing base oil, and a process for their preparation.

High aromatic mineral oils are used in the production of rubber compositions such as natural rubbers and synthetic rubbers because of their high affinity with rubber components and excellent processability, softness, and economy of rubber compositions. For example, synthetic rubbers such as SBR are blended with extender oil (extender oil) at the time of synthesis, and rubber processed products such as tires are blended with processing oil (for example, Process oil) (see, for example, Patent Document 1).

In Europe, on the other hand, regulations requiring that DMSO extracts or specific carcinogenic polycyclic aromatic compounds containing a certain amount or more are not to be used in the manufacture of tires or tire parts have been adopted from 2010 onwards. As a result, the extractions obtained by extracting the reduced-pressure distillation oil with a polar solvent generally have a high polycyclic aromatic content and can not be used as a rubber compounding oil under the above-mentioned regulations. Therefore, a rubber compounding oil that meets these regulations is required.

As a rubber compounding oil conforming to such regulations, Patent Document 1 discloses a rubber compounding oil which has an aromatic hydrocarbon content (C _A ) of 20 to 35% by weight, a glass transition temperature (T _g ) of -55 to -30 캜 and a kinematic viscosity Based process oil having a polycyclic aromatic component amount (PCA) of 20 to 50 mm 2 / s and not more than 3% by weight of petroleum-based process oil. When the rubber obtained by blending this petroleum-based process oil with a diene rubber is used in a tire, it is possible to achieve both low fuel consumption and gripability, and it is possible to improve the heat aging resistance and the thermal abrasion resistance.

However, conventionally, a rubber compounding oil is known as a high aromatic containing base oil containing a reduced-pressure distillate fraction and solvent extraction extract of deasphalted oil (for example, Patent Document 2). Solvent extraction of decompression distillate oil Extracts generally contain many polycyclic aromatic components, and due to the above restrictions, it is becoming impossible to use them as a rubber compound oil in this state. As a technique for coping with such a situation, there is also known a method for improving the yield of extractions for the purpose of low aromaticization by hydrogenation treatment of aromatic compounds and dilution effect of polycyclic aromatics. However, in such a method, there is a fear that the economical efficiency due to the addition of the hydrogenation equipment, the lower aromatization, or the yield of the lubricating base oil which is a by-product deteriorates.

On the other hand, rubber compounding oils are required to have a high flash point (250 DEG C or higher) which is outside the scope of dangerous article fourth petroleum products in order to improve handling and handling properties.

In addition, rubber compounded oils are required to lower the glass transition point in order to improve the low temperature properties (low temperature elastic modulus and the like) of the rubber. For example, Patent Documents 1 and 3 propose a rubber compounding oil having a low glass transition point of -55 to -30 占 폚 and -45 to -20 占 폚, respectively.

However, in general, it is generally difficult to satisfy both the high aromatic content and the low glass transition point because the glass transition point and the aromatic content show opposite characteristics. For example, a rubber blend oil having an aromatic content of 50% by mass or more according to ASTM D 2007 and having a glass transition point of -45 캜 or less is not obtained (see, for example, Example of Patent Document 3, Comparative Example). Further, as the glass transition point of the rubber compounding oil is lowered, not only the aromatic component but also the flash point tends to be lowered.

Here, the high aromatic containing base oil containing the conventional crude extract has a high pour point and a high glass transition point. Further, the lubricating base oil obtained by purifying raffinate obtained by extracting the reduced-pressure distillate fraction by polar solvent extraction has a low pour point, but has a low aromatic content and high aniline point. Therefore, the lubricating base oil used for the extractant oil used for the production of SBR and the like It is difficult.

As a method for producing the non-halogenated rubber compounded oil, for example, a method of producing (1) a method of hydrogenating the extract to reduce polycyclic aromatics, and (2) A method of diluting polycyclic aromatics by increasing the yield, and a method of producing (3) a method of performing solvent extraction of the reduced-pressure distillate fraction in two steps (Patent Document 2).

In addition, as such an aromatic-containing base oil, when the flash point is 250 ° C or higher, it is required to have a high flash point because it becomes outside of the object of the dangerous article fourth petroleum and is easy to handle. In addition, rubber compound induction with a low glass transition point has been proposed (for example, Patent Documents 1 and 3).

Of these, Patent Document 1 discloses a rubber compounded oil blended with a diene rubber, which has an aromatic hydrocarbon content (C _A ) of 20 to 35% by weight, a glass transition temperature (T _g ) of -55 to -30 캜, 100 ° C) of 20 to 50 mm 2 / s and a polycyclic aromatic component amount (PCA) of 3% by weight or less. When the rubber obtained by blending this petroleum-based process oil with a diene rubber is used in a tire, it is possible to achieve both low fuel consumption and gripability, and it is possible to improve the heat aging resistance and the thermal abrasion resistance.

Japanese Laid-Open Patent Publication No. 2004-155959 Japanese Patent Publication No. 3658155 Japanese Patent Application Laid-Open No. 97/35462

However, in the production method (1), the aromatic content of the product obtained tends to decrease with the deterioration of the economical efficiency accompanying the addition of the hydrogenation equipment. In the production method (2), the lubricating oil The yield of the base oil is lowered and the aromatic content thereof is also lowered. Even in the production method (3), although the density is less than 0.94 g / cm < 3 >, the polycyclic aromatics are few and the yield of the extract of the high aromatics is increased, the yield of raffinate is largely lowered and the aromatic content thereof is also lowered have.

From the raffinate and extract obtained by the polar solvent extraction method using the reduced-pressure distillate oil as the raw material as described above, it is possible to obtain a product having a high flash point and a low glass transition point, a high total aromatic content and a sufficient specific carcinogenic polycyclic aromatic compound A process for producing a reduced aromatic base-containing base oil at a high yield is not known. In particular, a non-vulcanizable aromatic-containing base oil obtained from raffinate, which is also useful as a rubber compounding oil or a base material thereof and as a lubricating oil base oil, while obtaining a non-cancerous high aromatic base oil obtained from a rubber compounding oil or an extract thereof useful as a base thereof The method of obtaining the compound at a high yield is not known.

Therefore, the present invention provides a rubber compounded oil having a high flash point and a low glass transition point while sufficiently keeping the total aromatic content high, and a content of a specific polycyclic aromatic compound being sufficiently reduced, and a process for producing such a rubber compounded oil 1 Purpose.

The present invention also relates to a process for producing polylactic acid from raffinate and extract obtained by a polar solvent extraction method using a reduced-pressure distillate as a raw material and having a high flash point, a low glass transition point, a high total aromatic content, It is a second object of the present invention to provide an aromatic-containing base oil which is sufficiently reduced and to provide a process for producing an aromatic base oil capable of producing such an aromatic base oil at a high yield.

(A) a total aromatic content of 50 mass% or more according to ASTM D 2007 or ASTM D 2549, a flash point of 250 ° C or more, a difference between a pour point and a glass transition point of 45 ° C or more, A pyrene content of 1 mass ppm or less, and a total content of the specific aromatic compounds of the following 1) to 8) is 10 mass ppm or less.

1) benzo (a) pyrene (BaP)

2) benzo (e) pyrene (BeP)

3) Benzo (a) Anthracene (BaA)

4) Chrysene (CHR)

5) benzo (b) fluoransen (BbFA)

6) Benzo (j) Fluorans (BjFA)

7) benzo (k) fluoransen (BkFA)

8) dibenzo (a, h) anthracene (DBAhA)

The rubber compounded oil of the present invention has a high flash point and a low glass transition point while keeping the total aromatic content high, and at the same time, the content of the specific polycyclic aromatic compound is sufficiently reduced.

The rubber compounded oil of the present invention contains raffinate or its refined oil obtained by separating the reduced pressure distillate fraction of the crude residue of the atmospheric distillation residue in the solvent extraction step and has a kinematic viscosity at 40 DEG C of 60 to 600 mm < 2 > / s, aniline point above 70 ℃, 10% point of 400 to 500 ℃, aromatic base stocks contain less than 90% points from 500 to 600 ℃, the% C _a by the ASTM D 3238 3 to 20, a glass transition point of -30 ℃ by GC distillation ( a), and an extractant or a refined oil obtained by separating the reduced-pressure distillate fraction of the atmospheric distillation residue from the solvent extraction process, wherein the composition has a kinematic viscosity at 40 ° C of 200 mm 2 / s or more, an aniline point of 90 ° C or less, Containing base oil (b) among the aromatic-containing base oils (b) having a density of not less than 0.94 g / cm 3 and a total aromatic content of not less than 30 mass% according to ASTM D 2549, When the content is 95% by mass or less and the direction It contains the content of the base oil (b) at least 5% by weight is preferred.

In the present invention, the solvent extraction step may be a step of bringing the reduced-pressure distillate fraction and the polar solvent into contact with each other in a first extraction column having a column bottom temperature of 30 to 90 ° C and a column top temperature higher than the column bottom temperature, A first solvent extraction step of obtaining a first extract and a first extraction step in which a first raffinate and a polar solvent are brought into contact with each other in a second extraction column wherein the column bottom temperature and the column top temperature are respectively 10 ° C or more higher than the first extraction column, And a second solvent extraction step of obtaining a second extract and a second solvent extraction step, and the aromatic-containing base oil (b) preferably contains a second extract or a refined oil thereof.

Further, the present invention is characterized in that it contains raffinate or a refined oil obtained by separating the reduced-pressure distillation oil of the crude oil at the solvent extraction step and has a kinematic viscosity at 40 DEG C of 60 to 600 mm2 / s, Containing base oil (a) having a glass transition point of at least 70 ° C, a 10% point by GC distillation of 400 to 500 ° C, a 90% point of 500 to 600 ° C, a% C _A of 3 to 20 according to ASTM D 3238, , And an extractant or its refined oil obtained by separating the reduced-pressure distilled oil fraction of the atmospheric distillation residue oil in a solvent extraction process, and has a kinematic viscosity at 40 ° C of 200 mm 2 / s or more, an aniline point of 90 ° C or less, Containing base oil (b) having a density of 0.94 g / cm 3 or more and a total aromatic content of 30% by mass or more according to ASTM D 2549, and the total aromatic content according to ASTM D 2007 or ASTM D 2549 is 50 mass% %, Flash point (A) the pyrene content is 1 mass ppm or less, and the total content of the specific aromatic compounds in the following 1) to 8) is 10 mass ppm or less , And the content of the aromatic containing base oil (a) is more than 0 mass% and not more than 95 mass%, and the content of the aromatic containing base oil (b) is less than 5 mass% and less than 100 mass%.

1) benzo (a) pyrene (BaP)

2) benzo (e) pyrene (BeP)

3) Benzo (a) Anthracene (BaA)

4) Chrysene (CHR)

5) benzo (b) fluoransen (BbFA)

6) Benzo (j) Fluorans (BjFA)

7) benzo (k) fluoransen (BkFA)

8) dibenzo (a, h) anthracene (DBAhA)

The rubber blend oil obtained by the production method of the present invention has a high flash point and a low glass transition point while sufficiently keeping the total aromatic content, and the content of the specific polycyclic aromatic compound is sufficiently reduced. The rubber compounded oil containing the aromatic-containing base oil (b) of the present invention is characterized in that the difference between the pour point and the glass transition point is 45 占 폚 or higher, particularly 60 占 폚 or higher, so that the total aromatic content is 50% A rubber blend oil having a glass transition point of -45 캜 or lower can be obtained even if the pour point is 15 캜 or higher. Further, since the aromatic-containing base oil (b) does not need to be subjected to a treatment such as a dewaxing treatment or a hydrogenation treatment, it is also excellent in economy.

In a second aspect of the present invention, in the first extraction column, the bottoms temperature is from 30 to 90 DEG C and the top temperature is higher than the bottoms temperature, the reduced-pressure distillation oil fraction of the atmospheric distillation residue of the crude oil and the polar solvent are brought into contact with each other, A first solvent extracting step of obtaining raffinate and a first extract; and a step of bringing the first raffinate and the polar solvent into contact with each other in a second extraction column having a column bottom temperature and a column top temperature of 10 ° C or more higher than those of the first extraction column , A second solvent extraction step of obtaining a second extract having a density of 0.94 g / cm 3 or more at 15 캜 and a total aromatic content of 30 mass% or more at the second raffinate, and a second solvent extraction step Containing base oil containing at least a part of its refined oil and having a total aromatic content of 30 mass% or more.

According to the present invention, it is possible to produce an aromatic-containing base oil having a high flash point, a low glass transition point, a high total aromatic content and a sufficiently reduced content of a specific carcinogenic substance at a high yield. Such an aromatic containing base oil can be suitably used as a rubber compounded oil or as a raw material thereof.

The present invention relates to a process for producing a base oil, which comprises a base oil preparation step of subjecting a second raffinate to a refining treatment including a dewaxing treatment after the second solvent extraction step to obtain the refined oil, It is preferable to prepare an aromatic-containing base oil having a viscosity of 90 ° C or higher, a viscosity index of 90 ° C or higher, and a flash point of 250 ° C or higher.

In the present invention, it is preferable that after the second solvent extraction step, the second raffinate is subjected to a refining treatment including a dewaxing treatment to obtain refined oil, which contains refined oil and has kinematic viscosity at 40 DEG C of 60 to 120 mm < / s, and 10% by gas chromatography distillation at 400 to 460 ° C and 90% point at 500 to 540 ° C.

In the present invention, it is preferable that after the second solvent extraction step, the second raffinate is subjected to a refining treatment including a dewaxing treatment to obtain refined oil, which contains refined oil and has a kinematic viscosity at 40 DEG C of 120 to 250 < / s, and 10% by gas chromatography distillation at 450 to 520 ° C and 90% point at 540 to 600 ° C.

The aromatic containing base oil obtained by the production method of the present invention contains at least a part of the second extract and has a kinematic viscosity at 40 ° C of not less than 200 mm 2 / s, a flash point of not less than 250 ° C, a pour point of not more than 30 ° C, The glass transition point is -30 占 폚 or less, and the difference between the pour point and the glass transition point is 50 占 폚 or more. Further, the aromatic-containing base oil may be composed of the second extract.

The aromatic containing base oil obtained by the production method of the present invention contains at least a part of the second extract and has a dynamic viscosity at 40 캜 of not less than 200 mm 2 / s and less than 500 mm 2 / s, and a glass transition point of -60 To -40 < 0 > C. Such aromatic containing base oils include, for example, natural rubbers (NR), various butadiene rubbers (BR), various styrene-butadiene copolymer rubbers (SBR), polyisoprene rubbers (IR), butyl rubbers (BR) It can be suitably used particularly as a petroleum-based process oil or an extender oil blended with a diene rubber such as rubber, especially a diene rubber containing at least one styrene-butadiene copolymer rubber. Further, the aromatic-containing base oil may be composed of the second extract.

The aromatic-containing base oil obtained by the production method of the present invention preferably contains at least a part of the second extract, preferably has a kinematic viscosity at 40 캜 of 500 mm 2 / s or higher and a glass transition point of -50 캜 to -30 캜 Do. Such an aromatic-containing base oil can be suitably used, for example, as a petroleum-based process oil or an extender oil blended with the diene rubber as described above. Further, the aromatic-containing base oil may be composed of the second extract.

The aromatic-containing base oil obtained by the production process of the present invention has a benzo (a) pyrene content of 1 mass ppm or less and a total content of the specific aromatic compounds 1) to 8) shown below as 10 mass ppm or less desirable.

1) benzo (a) pyrene (BaP)

2) benzo (e) pyrene (BeP)

3) Benzo (a) Anthracene (BaA)

4) Chrysene (CHR)

5) benzo (b) fluoransen (BbFA)

6) Benzo (j) Fluorans (BjFA)

7) benzo (k) fluoransen (BkFA)

8) dibenzo (a, h) anthracene (DBAhA)

Such an aromatic-containing base oil can be suitably used as a petroleum-based process oil or an extender oil of a rubber-processed product such as a tire or a base thereof, since the content of a specific carcinogenic polycyclic aromatic compound is sufficiently reduced.

Further, the present invention provides an aromatic containing base oil obtained by a production method having the above-mentioned characteristics. This aromatic-containing base oil has a high flash point, a low glass transition point, a high total aromatic content and a sufficiently reduced content of carcinogenic substances, and has excellent properties as a petroleum-based process oil or extractor oil or its base material, Is also excellent.

Further, the present invention provides, in a third aspect, a rubber blend oil containing an aromatic containing base oil having the above characteristics.

According to the present invention, it is possible to provide a rubber blend oil having a high flash point and a low glass transition point while sufficiently reducing the content of a specific polycyclic aromatic compound while maintaining a high aromatic content, and a process for producing such rubber blended oils.

The rubber compounded oil of the present invention is highly compatible with rubber or rubber materials such as styrene-butadiene rubber because of its high aromatic content. When rubber is used as a rubber or rubber material such as a styrene-butadiene rubber having a glass transition point of about -57 to -44 占 폚, for example, or as a processed oil, a rubber excellent in low temperature characteristics can be produced. In addition, since the content of the polycyclic aromatic compound having a high flash point and carcinogenic properties is sufficiently reduced, safety is also high. In particular, as in Patent Document 1, when the aromatic hydrocarbon content (C _A ) is 20 to 35 mass% (C _{A according} to ASTM D 3238 agrees with 20 to 35) and the glass transition temperature (T _g ) (BR), various styrene-butadiene copolymer rubber (SBR), poly (styrene-butadiene rubber), and polybutylene terephthalate Butadiene rubber (IR), butyl rubber (BR), and arbitrary blend rubbers thereof, in particular a styrene-butadiene copolymer rubber, and the rubber obtained thereby is used as a tire Fuel ratio and gripability can be achieved at the same time, and the heat aging resistance and the heat abrasion resistance can be improved.

Further, according to the present invention, the raffinate and extract obtained by the polar solvent extraction method using the reduced-pressure distillate oil as a raw material have high flash point, low glass transition point, high total aromatic content, It is possible to provide a sufficiently reduced aromatic containing base oil. It is also possible to provide a process for producing an aromatic-containing base oil capable of producing such an aromatic base oil at a high yield.

BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a process drawing showing a suitable embodiment of a process for producing rubber compounding oil according to the present invention. Fig.

Best Mode for Carrying Out the Invention Hereinafter, preferred embodiments of the present invention will be described with reference to the drawings. The rubber blend oil of the present embodiment is excellent in affinity with rubber, softening property, flash point and safety, and also has a high level of characteristics of rubber composition such as low fuel consumption, gripability, heat aging resistance and heat abrasion resistance It is preferable to have the following properties.

Is usually 50 to 90% by mass, preferably 55% by mass or more, more preferably 57% by mass or more, particularly preferably 60% by mass or more, and preferably 80% by mass or more, based on ASTM D 2007 (clay gel method) By mass or less, more preferably 70% by mass or less.

Is usually 5 to 50% by mass, preferably 10% by mass or more, more preferably 20% by mass or more, preferably 40% by mass or less, more preferably 30% by mass or less, % Or less.

The amount of the polar compound by ASTM D 2007 (clay gel method) is usually 1 to 20 mass%, preferably 2 mass% or more, more preferably 5 mass% or more, and preferably 15 mass% or less, 12 mass% or less, and more preferably 10 mass% or less.

The ratio of the saturated component / polar compound component by ASTM D 2007 (clay gel method) is usually 0.25 to 50, preferably 1 or more, more preferably 2.5 or more, further preferably 3 or more, and preferably 20 or less , More preferably 10 or less, and further preferably 5 or less.

The content of the benzo (a) pyrene (BaP) is 1 mass ppm or less, and the total content of the specific aromatic compounds (PAH) 1) to 8) shown below is 10 mass ppm or less. This makes it possible to sufficiently reduce the risk of carcinogenicity and to provide a rubber compounding oil with higher safety.

1) benzo (a) pyrene (BaP)

2) benzo (e) pyrene (BeP)

3) Benzo (a) Anthracene (BaA)

4) Chrysene (CHR)

5) benzo (b) fluoransen (BbFA)

6) Benzo (j) Fluorans (BjFA)

7) benzo (k) fluoransen (BkFA)

8) dibenzo (a, h) anthracene (DBAhA)

The benzo (a) pyrene in the present specification means the benzo (a) pyrene (BaP) in the above 1), and the specific aromatic compound means the aromatic compound (PAH) in the above 1) to 8). These specific aromatic compounds can be quantitatively analyzed by GC-MS analysis after preparing a sample to which an internal standard substance is added after separating and concentrating the target component.

The flash point is 250 占 폚 or higher, preferably 260 占 폚 or higher, more preferably 280 占 폚 or higher, preferably 350 占 폚 or lower, more preferably 320 占 폚 or lower, still more preferably 310 占 폚 or lower. The flash point in the present specification means a flash point by Cleveland Open Type (COC) measured in accordance with JIS K 2265.

The difference between the pour point and the glass transition point is preferably 45 占 폚 or higher, preferably 50 占 폚 or higher, more preferably 60 占 폚 or higher, further preferably 65 占 폚 or higher, preferably 100 占 폚 or lower, more preferably 80 占 폚 or lower to be.

The pour point is preferably 30 占 폚 or lower, more preferably 25 占 폚 or lower, preferably -10 占 폚 or higher, more preferably 5 占 폚 or higher, further preferably + 10 占 폚 or higher, particularly preferably +12.5 占 폚 or higher to be. In this specification, the pour point means a pour point measured in accordance with JIS K 2269.

A glass transition point (T _g) is preferably below -30 ℃, more preferably at most -40 ℃, more preferably not more than -45 ℃, more preferably preferably less than -48 ℃, in particular than the - 50 ° C or lower, preferably -80 ° C or higher, more preferably -60 ° C or higher, and still more preferably -55 ° C or higher.

In the present specification, "glass transition point (T _g)" is, obtained from the amount of heat change in peak in the glass transition region, which is measured when the temperature was raised in a DSC (differential scanning calorimetry) at a constant rate of temperature increase (10 ℃ / min) ≪ / RTI > The initial temperature is usually set at a temperature of about 30 to 50 DEG C or lower than the predicted glass transition point, the temperature is kept at the initial temperature for a certain period of time, and then the temperature is raised. Specifically, in the present embodiment, measurement can be made under the following conditions.

Apparatus: Thermal analysis system DSC Q100 manufactured by T.A.

Initial temperature: -90 ° C, hold for 10 minutes

Heating rate: 10 ° C / min

End temperature: 50 ° C, hold for 10 minutes

Further, the method of calculating the glass transition point from the peak of the change in the amount of heat can be determined by the method described in JIS K 7121.

The density at 15 占 폚 is usually 0.9 g / cm3 to 1.0 g / cm3, preferably 0.94 g / cm3 or more, more preferably 0.945 g / cm3 or more, preferably 0.98 g / cm3 or less Lt; 3 > / cm < 3 >

The kinematic viscosity at 40 캜 is usually 200 to 3000 mm 2 / s, preferably 300 mm 2 / s or more, more preferably 400 mm 2 / s, further preferably 500 mm 2 / s or more, / s or less, more preferably 1000 mm2 / s or less, and further preferably 800 mm2 / s or less. In the present specification, the kinematic viscosity at each temperature means the kinematic viscosity at each temperature measured in accordance with JIS K 2283.

The kinematic viscosity at 100 占 폚 is usually 10 to 100 mm2 / s, more preferably 15 mm2 / s or more, further preferably 20 mm2 / s or more, preferably 60 mm2 / s or less, S2 / s, more preferably not more than 32 mm2 / s.

The aniline point is usually 50 to 100 ° C, preferably 60 ° C or more, more preferably 65 ° C or more, further preferably 70 ° C or more, preferably 90 ° C or less, more preferably 85 ° C or less . In the present specification, the aniline point means an aniline point measured in accordance with JIS K 2256-1985.

The nitrogen content is usually 0.01 to 0.2 mass%, preferably 0.03 mass% or more, more preferably 0.05 mass% or more, preferably 0.15 mass% or less, and more preferably 0.1 mass% or less. In the present specification, the nitrogen content means the nitrogen content by the chemiluminescence method measured in accordance with JIS K 2609.

% C _N is usually 5 to 30, preferably 10 or more, more preferably 14 or more, preferably 25 or less, more preferably 20 or less. % C _A is usually 10 to 40, preferably 17 or more, more preferably 20 or more, preferably 35 or less, more preferably 30 or less, still more preferably 25 or less. % C _P is usually 30 to 85, preferably 40 or more, more preferably 50 or more, preferably 73 or less, more preferably 66 or less. The% C _P ,% C _N and% C _A in the present specification are calculated by the method according to ASTM D 3238-85 (ndM ring analysis), except that the content of paraffin The percentage of the number of carbon atoms to the total number of carbon atoms, the percentage of the total number of naphthenic carbon atoms to the total number of carbon atoms, and the percentage of the aromatic carbon atoms to the total number of carbon atoms.

The total aromatic content is usually 30 to 90 mass%, preferably 40 mass% or more, more preferably 50 mass% or more, preferably 80 mass% or less, and more preferably 70 mass% or less. In the present specification, the term "whole aromatic fraction" means a content of an aromatic fraction measured in accordance with ASTM D 2007 or ASTM D 2549, unless otherwise specified.

The rubber compounding oil of the present embodiment contains raffinate or its refined oil obtained by separating the reduced-pressure distillation oil fraction of the atmospheric distillation residue of crude oil in the solvent extraction step and has a kinematic viscosity at 40 ° C of 60 to 600 mm 2 / s , An aniline point of 70 ° C or higher, a 10% point by GC distillation of 400 to 500 ° C, a 90% point of 500 to 600 ° C, a% C _A of 3 to 20 according to ASTM D 3238 and a glass transition point of -30 ° C or lower (A) obtained by separating the reduced-pressure distillation residue of an atmospheric distillation residue and a refined oil obtained by separating the distillation residue of the reduced-pressure distillation residue in a solvent extraction process, and has a kinematic viscosity at 40 ° C of not less than 200 mm 2 / s, Containing base oil (b) having an aniline point of 90 占 폚 or less, a density at 15 占 폚 of 0.94 g / cm3 or more, and a total aromatic content by ASTM D 2549 of 30 mass% or more. Hereinafter, the aromatic containing base oil (a) (hereinafter referred to as base oil (a)) and the aromatic containing base oil (b) (hereinafter referred to as base oil (b)) will be described.

The base oil (a) is obtained by bringing the reduced-pressure distillate fraction of crude distillation residue of crude oil into contact with a polar solvent in a first extraction column having a column bottom temperature of 30 to 90 ° C and a column top temperature higher than the column bottom temperature, And a second extraction column in which the column bottom temperature and the column top temperature are respectively higher than the first extraction column by at least 10 ° C and the first raffinate is brought into contact with the polar solvent, And the second raffinate obtained by the second solvent extraction step to obtain a second extract having a density of 0.94 g / cm 3 or more at 15 ° C and a total aromatic content of 30 mass% or more, Containing base oil is 30 mass% or more.

The base oil (a) is an aromatic base oil obtained by subjecting a second raffinate to a refining treatment including a dewaxing treatment, wherein kinematic viscosity at 40 ° C is 60 to 120 mm 2 / s, 10% by GC distillation is 400 (A1) and / or a kinematic viscosity at 40 DEG C of 120 to 250 mm < 2 > / s, 10% point by GC distillation of 450 to 520 DEG C and 90% point of 540 to 600 DEG C Lt; 0 > C (a2).

The base oil (b) preferably has a kinematic viscosity at 40 ° C of at least 200 mm 2 / s, a flash point of at least 250 ° C, a pour point of at most 30 ° C, an aniline point of at most 90 ° C, Containing base oil having a glass transition point difference of 45 占 폚 or higher.

(B1) having a kinematic viscosity at 40 DEG C of less than 500 mm < 2 > / s and a glass transition point of from -60 to -40 DEG C and / or a kinematic viscosity at 40 DEG C of 500 mm & / s, and the glass transition point is -50 to -30 占 폚.

Preferable properties of the base oil (a) and base oil (b) will be described in detail.

The pour point of the base oil (a) is preferably -10 ° C or lower, and may be lower than -20 ° C. However, the pour point of the base oil (a) is more preferably -10 to -20 占 폚, from the viewpoint of production cost of the rubber compounded oil. By using the base oil (a) having a pour point of -10 占 폚 or lower, a rubber compounded oil having a lower glass transition point can be easily obtained.

The glass transition point of the base oil (a) is preferably -30 占 폚 or lower, more preferably -50 占 폚 or lower, preferably -100 占 폚 or higher, more preferably -80 占 폚 or higher, even more preferably -70 Lt; / RTI > When the glass transition point is too high, it tends to make it difficult to obtain a rubber blend oil having a low glass transition point. When the glass transition point is too low, the blend condition tends to be excessively strict, and thus the production cost tends to increase.

The aniline point of the base oil (a) is preferably 70 占 폚 or higher, more preferably 90 占 폚 or higher, and still more preferably 100 占 폚 or higher. Is preferably 120 占 폚 or lower from the viewpoint of making it easy to prepare a rubber compounded oil having an aniline point that is excellent in compatibility with rubber and maintains the properties of the rubber composition.

As the composition of the base oil (a),% C _A is preferably 3 to 20, more preferably 5 to 10, and% C _N is preferably 15 to 35, more preferably 20 to 30. The% C _P in the base oil (a) is determined according to% C _A ,% C _N , preferably 45 to 82, more preferably 60 to 75, still more preferably 65 to 70. By using the base oil (a) having the composition within the above range, it is possible to easily produce a rubber compounding oil having a composition which is excellent in compatibility with rubber and has a proper composition for maintaining the properties of the rubber composition.

The nitrogen content of the base oil (a) is preferably 0.01 mass% or less, more preferably 0.008 mass% or less, and less than 0.001 mass%. However, the use of a low-refining lubricating base oil can reduce the manufacturing cost of the rubber compounded oil, and is preferably 0.002 mass% or more, and more preferably 0.003 mass% or more from the viewpoint of economy.

The flash point of the base oil (a) is 250 占 폚 or higher, preferably 255 占 폚 or higher, from the viewpoint that the flash point of the rubber compounding oil is 250 占 폚 or higher, The flash point of the base oil (b) can also be increased, so it is not necessary to raise the flash point of the base oil (a) more than necessary, preferably 290 ° C or lower, more preferably 280 ° C or lower.

The 90% point in the GC distillation of the base oil (a) is 500 ° C or higher, and preferably 500 to 600 ° C. As the base oil (a1), which is one type of the base oil (a), those having a temperature of 510 to 550 ° C and a base oil (a2) of another form of the base oil (a), those having a temperature of 550 to 590 ° C can be used. There is no particular limitation on the 10% point in the GC distillation of the base oil (a), and from the viewpoint that the flash point of the rubber compounding oil is 250 DEG C or higher, Deg.] C, preferably 440 to 500 [deg.] C. As the base oil (a1), 10% point in the GC distillation is from 440 to 470 DEG C, and base oil (a2) having a 10% point in the GC distillation is 450 to 500 DEG C can be used.

The base oil (a) preferably has a content of 1) benzo (a) pyrene (BaP) of 1 mass ppm or less and a total content of the specific aromatic compound (PAH) of 1) to 8) Or less. This makes it possible to produce a rubber compounding oil in which the carcinogenicity is sufficiently reduced and the safety is higher.

The kinetic viscosity of the base oil (a) at 40 캜 is preferably 60 to 600 mm 2 / s, more preferably 60 to 300 mm 2 / s, and still more preferably 70 to 200 mm 2 / s.

When a base oil (b) having a kinematic viscosity at 40 DEG C of less than 2000 mm < 2 > / s is used, the kinematic viscosity at 40 DEG C is preferably 50 to 500 mm < 2 & (A1) of 60 to 80 mm 2 / s and / or a base oil (a2) of 120 to 250 mm 2 / s is preferably used.

The total aromatic content of the base oil (a) is not particularly limited and is usually 20 mass% or more, preferably 30 mass% or more, more preferably 35 mass% or more, preferably 50 mass% or less, And not more than 45% by mass. If the total aromatic content of the base oil (a) is less than 20% by mass, it tends to be difficult to obtain a rubber compounding oil having a high aromaticity. On the other hand, when the total aromatic content of the base oil (a) is more than 50 mass%, oxidation stability in the case of using as a lubricating oil base oil is lowered and it becomes difficult to be used both as a lubricant base oil and a rubber compounding oil. Is lowered.

The aniline point of the base oil (b) is preferably 40 to 90 占 폚, more preferably 45 to 70 占 폚, and still more preferably 50 to 65 占 폚. If the aniline point is within this range, a rubber compounding oil having an aniline point that is excellent in compatibility with the rubber and maintains the properties of the rubber composition can be easily produced even if a lubricant base oil having a high aniline point is blended.

As the composition of the base oil (b),% C _A is preferably 25 to 45, more preferably 30 to 40, and% C _N is preferably 5 to 20, more preferably 6 to 12. Further,% C _P is determined according to% C _A ,% C _N , preferably 35 to 70, more preferably 48 to 64. If the composition of the base oil (b) is within the above range, even if the base oil (a) having a high paraffin property is blended, a rubber blend oil having excellent compatibility with rubber and having a composition suitable for maintaining the properties of the rubber composition can be easily produced can do.

The nitrogen content of the base oil (b) is preferably 0.01 mass% or more, more preferably 0.05 mass% or more, still more preferably 0.1 mass% or more, and particularly preferably 0.15 mass% or more. The higher nitrogen content of the base oil (b) means that the nitrogen content of the raffinate obtained by the solvent extraction process is lowered and the refining degree of the lubricating base oil is improved. Therefore, the use of the base oil (b) having a high nitrogen content as the rubber compounding oil is preferable in that the entire reduced-pressure distillate fraction can be used effectively.

The pour point of the base oil (b) is preferably 30 占 폚 or lower, more preferably 25 占 폚 or lower. The pour point of the base oil (b) is preferably 5 占 폚 or higher, more preferably 10 占 폚 or higher, still more preferably 15 占 폚 or higher, particularly preferably 20 占 폚 or higher.

The base oil (b) may be a crude extract having a high pour point, and preferably has a low glass transition point. The difference between the pour point of the base oil (b) and the glass transition point (pour point-glass transition point) is preferably not lower than 45 ° C, more preferably not lower than 50 ° C, even more preferably not lower than 55 ° C, Or higher, preferably 100 ° C or lower, and more preferably 80 ° C or lower.

The glass transition point of the base oil (b) is preferably -30 占 폚 or lower, and preferably -60 占 폚 or higher. The glass transition point of the aromatic containing base oil (b1), which is one type of base oil (b), is from -60 to -40 占 폚, and the glass transition point of the other type of aromatic containing base oil (b2) is from -50 to -30 占 폚.

The base oil (b) is preferably such that the content of 1) benzo (a) pyrene (BaP) is 1 mass ppm or less, and the content of the specific aromatic compound (PAH) in the above 1) And preferably 10 mass ppm or less. This makes it possible to produce a rubber compounding oil in which the carcinogenicity is sufficiently reduced and the safety is higher.

The flash point of the base oil (b) is not particularly limited, but it is preferably not lower than 250 ° C, more preferably not lower than 270 ° C, more preferably not lower than 250 ° C, more preferably not lower than 250 ° C, Preferably 290 DEG C or higher, particularly preferably 300 DEG C or higher.

The total aromatic content of the base oil (b) is preferably 30 mass% or more, more preferably 50 mass% or more, still more preferably 55 mass% or more, particularly preferably 60 mass% or more, Preferably 65 mass% or more, preferably 90 mass% or less, more preferably 80 mass% or less, further preferably 75 mass% or less.

When the total aromatic content of the base oil (b) is less than 50 mass%, it tends to be difficult to obtain a rubber compounding oil having a high aromatic content. When the total aromatic content exceeds 90 mass%, the yield of the extract tends to deteriorate, It is not preferable in view of the above.

Next, a preferred embodiment of the process for producing the rubber compounded oil of the present invention will be described.

The present embodiment has a first solvent extraction step and a second solvent extraction step for producing the base oil (a) and the base oil (b), and a blending step for blending the produced base oil (a) and base oil (b). First, the first solvent extraction step and the second solvent extraction step for producing the base oil (a) and the base oil (b) will be described.

The first solvent extracting step is a step of bringing the distillation distillate fraction of the atmospheric distillation residue of the crude oil and the polar solvent into contact with each other in a first extraction column having a column bottom temperature of 30 to 90 ° C and a column top temperature higher than the column bottom temperature, A first extract is obtained. In the second solvent extraction step, the first raffinate and the polar solvent are brought into contact with each other in a second extraction column having a column top temperature and a column top temperature higher than the first extraction column by 10 ° C or more, respectively, Is not less than 0.94 g / cm 3 and the total aromatic content is not less than 30 mass%. Hereinafter, the details of each step will be described.

(First solvent extraction step)

BRIEF DESCRIPTION OF DRAWINGS FIG. 1 is a process diagram for explaining a first solvent extraction process and a second solvent extraction process in the method for producing a rubber compounded oil in the present embodiment. FIG. In the first solvent extraction step, first, the reduced-pressure distillate fraction of the crude residue of the atmospheric distillation residue is introduced into the first extraction column 30 having a column bottom temperature of 30 to 90 ° C and a column top temperature higher than the column bottom temperature, To separate the first raffinate and the first extract. The polar solvent is supplied from the pipe 34 to the first extraction column 30. On the other hand, the reduced-pressure distillate fraction is supplied to the first extraction tower 30 through the pipe 16.

The reduced-pressure distillate fraction is an oil fraction obtained by introducing an ordinary-pressure distillation residue of crude oil into a vacuum distillation apparatus. The reduced-pressure distillate fraction is not particularly limited, and may be any of a light lubricating oil fraction, a medium quality lubricating oil fraction, a heavy lubricating oil fraction, or a mixture thereof, or a reduced-pressure distillation fraction. Is preferably 200 to 1,500 N, more preferably 250 to 1,200 N, in view of increasing the flash point of the finally obtained aromatic containing base oil and obtaining an aromatic containing base oil having an appropriate viscosity range without excessively increasing the viscosity Lt; RTI ID = 0.0 > 600 < / RTI > In this specification, "N" means a neutral oil obtained from reduced pressure distillation oil. For example, if the viscosity is 300 N, the viscosity at 100 ° F (37.8 ° C.) is 300 seconds bolt universal primary (SUS) .

In the present embodiment, it is preferable to select the reduced-pressure distillate fraction so that the base oil (a) has a viscosity of 200 to 1500 N, preferably 250 to 600 N or 600 to 1200 N, more preferably 300 to 450 N or 700 to 1000 N.

The column bottom temperature of the first extraction column 30 used in the first solvent extraction step is 30 to 90 占 폚, preferably 50 to 70 占 폚, and more preferably 55 to 65 占 폚. The topping temperature of the first extraction column 30 is preferably higher than the column bottom temperature, preferably 10 to 50 占 폚, more preferably 15 to 40 占 폚, and still more preferably 25 to 35 占 폚. Concretely, the overhead temperature is preferably 60 to 120 占 폚, more preferably 80 to 100 占 폚, and still more preferably 85 to 95 占 폚.

The solvent ratio in the first solvent extraction step is preferably 0.5 to 3, more preferably 0.7 to 2, still more preferably 1 to 1.5. In the present specification, the term " solvent ratio " means the volume ratio of the solvent to the raw material (solvent capacity / raw material capacity).

Under the above conditions, the polar solvent and the reduced-pressure distillate fraction are in countercurrent contact with each other in the first extraction tower 30, and the first extracting column 30, A mixture of the solvent is obtained, and a mixture of the first raffinate and the polar solvent is obtained through the pipe 36 from the column top. Further, the mixture of the first extract and the polar solvent is classified into a first extract and a polar solvent in a sorting tower (not shown). In addition, the mixture of the first raffinate and the polar solvent may be classified into the first raffinate and the polar solvent in the classification tower (not shown), or may be introduced into the second extraction column 40 without being classified.

In the classification tower not shown, the polar solvent classified into the first extract and the first raffinate is recovered and reused. Examples of the polar solvent include polar solvents such as furfural, phenol, cresol, sulfolane, N-methylpyrrolidone, dimethylsulfoxide, formylmorpholine, and glycol solvents. In the present embodiment, it is preferable to use furfural in that a general lubricant base oil solvent extraction facility can be used as it is.

As described above, in the first solvent extraction step, the reduced-pressure distillate fraction is separated into the first raffinate and the first extract. The yield of the first raffinate obtained in the first solvent extraction step is preferably 50 to 90% by volume, more preferably 60 to 85% by volume, and still more preferably 70 to 80% by volume, Capacity%. The yield of the first extract obtained in the first solvent extraction step is preferably 10 to 50% by volume, more preferably 15 to 40% by volume, and still more preferably 20 to 30% by volume, based on the reduced- Capacity%.

Since the specific aromatic compound (PAH) to be described later is extracted by the first solvent extraction step on the side of the first extract, the second extract, the second raffinate, and the aromatic compounds of the aromatic containing base oils obtained therefrom (PAH) can be sufficiently reduced. Further, since the first extract contains a specific aromatic compound (PAH), it tends not to be suitable for a lubricating oil or a rubber compounding oil. Therefore, by making the yield of the first extract to, for example, not more than 30% by volume, it is possible to obtain the second raffinate and the second extract which are useful as the lubricating oil, the rubber compounding oil or the base material thereof in high yield. For example, the total amount of the second raffinate and the second extract may be 70% by volume or more based on the reduced-pressure distillate fraction, and the production method of the aromatic- It can be said that it is extremely useful in terms of.

In the second solvent extraction step, the first raffinate obtained in the first solvent extraction step or a mixture of the first raffinate and the polar solvent and the polar solvent is supplied from the pipe 36 and the pipe 44 to the second extraction tower 40 Respectively, and in the second extraction column 40, the first raffinate and the polar solvent are brought into contact with each other. The column bottom temperature and the column top temperature of the second extraction column (40) are respectively higher than those of the first extraction column (30) by 10 ° C or more.

The column bottom temperature of the second extraction column 40 used in the second solvent extraction process is 10 ° C or more higher than the column bottom temperature of the first extraction column 30 in the first solvent extraction process and is preferably 10 to 50 ° C More preferably 15 to 40 占 폚, and more preferably 20 to 30 占 폚. Specifically, the column bottom temperature of the second extraction column 40 is preferably 40 to 140 占 폚, more preferably 60 to 100 占 폚, and still more preferably 80 to 95 占 폚.

The topping temperature of the second extraction column 40 is preferably 10 to 50 占 폚 higher than the column bottom temperature, more preferably 15 to 40 占 폚, and still more preferably 25 to 35 占 폚. Specifically, the overhead temperature of the second extraction column 40 is preferably 50 to 150 占 폚, more preferably 80 to 140 占 폚, and still more preferably 110 to 130 占 폚.

The ratio of the solvent in the second solvent extraction step is preferably 1 to 4, more preferably 1.3 to 3.5, still more preferably 1.5 to 3.3. The ratio of the solvent in the second solvent extraction step is preferably at least 1.5 times the ratio in the first solvent extraction step.

Under the above conditions, the polar solvent and the first raffinate are countercurrently contacted in the second extraction column 40, and the second extraction column 40 passes through the pipe 48 from the bottom of the column of the second extraction column 40, A mixture of polar solvents is obtained, and a mixture of the second raffinate and the polar solvent is obtained from the tower through the pipe (46). The mixture of the second extract and the polar solvent is classified into a second extract and a polar solvent in a sorting tower not shown. Further, the mixture of the second raffinate and the polar solvent is classified into a second raffinate and a polar solvent in a classification tower not shown. In the classification tower not shown, the polar solvent separated from the second extract and the second raffinate is recovered and reused.

As described above, in the second solvent extraction step, the first raffinate is separated into the second raffinate and the second extract. The yield of the second raffinate obtained in the second solvent extraction step is preferably 50 to 90% by volume, more preferably 60 to 90% by volume, based on the first raffinate introduced into the second extraction column 40 85% by volume, more preferably 70 to 85% by volume. The yield of the second extract obtained in the second solvent extraction step is preferably 10 to 50% by volume, more preferably 15 to 40% by volume, and still more preferably 15 to 30% by volume.

In this embodiment, it is not necessary to use an individual extraction tower as the first and second extraction tows, and one extraction tower may be used as the first extraction tower 30 and the second extraction tower 40 as well. In this case, the raffinate obtained in the first solvent extraction step (preferably a polar solvent is removed) is once stored in a tank or the like, and the extraction condition is adjusted to the second extraction column 40 adjusted to the conditions of the second solvent extraction step And a second solvent extraction step may be carried out. In this way, excessive facility investment can be achieved.

By the second solvent extraction step, the first raffinate can be obtained with the second raffinate having a density of 0.94 g / cm 3 or more at 15 캜 and a total aromatic content of 30 mass% or more. When the density of the second extract at 15 캜 is 0.94 g / cm 3 or more, a tire using a diene rubber having a high aromatic content, a sufficiently low aniline point, a high flash point, and a large difference between a pour point and a glass transition point Based process oil or a base thereof in the production process of a rubber product or an extender oil or a base thereof in the process of producing a diene rubber. In addition, it is possible to obtain, from the second raffinate obtained at the same time, a high boiling aromatic base oil which is also useful as a base oil, a petroleum-based process oil, an extractor oil or a base material thereof having a total aromatic content of 30 mass% or more.

The density of the second extract at 15 캜 is preferably 0.94 g / cm 3 or more, more preferably 0.95 to 1 g / cm 3, and still more preferably 0.95 to 0.98 g / cm 3. The total aromatic content is preferably 30 mass% or more, more preferably 60 mass% or more, further preferably 80 mass% or more, and preferably 90 mass% or less. In the present specification, " total aromatic content " is a value measured in accordance with ASTM D 2549.

The second extract has a% C _A , as measured by ASTM D 2140, preferably 15 to 35, more preferably 20 to 33, and still more preferably 22 to 32.

It is preferable that this second extract has the following features.

ㆍ Flash point: preferably 250 占 폚 or higher, more preferably 260 占 폚 or higher, and preferably 310 占 폚 or lower.

Pour point: preferably 30 ° C or less, more preferably 10 to 30 ° C.

Aniline point: preferably 90 占 폚 or lower, more preferably 40 占 폚 to 80 占 폚, and still more preferably 50 占 폚 to 70 占 폚.

Glass transition point: preferably -30 占 폚 or lower, more preferably -40 占 폚 or lower, further preferably -60 占 폚 or higher.

Difference between the pour point and the glass transition point (pour point-glass transition point): preferably 45 ° C or more, more preferably 50 ° C or more, further preferably 55 ° C or more, preferably 100 ° C or less, Below 80 ℃.

ㆍ Benzo (a) Pyrene content: preferably 1 mass ppm or less.

The total content of the specific aromatic compound (PAH): preferably 10 mass ppm or less.

Next, a lubricating base oil which is a refined oil can be obtained by subjecting the second raffinate to a refining treatment comprising a dewaxing treatment by a dewaxing apparatus 50 and a hydrogenation finishing treatment by a hydrogenation finishing apparatus 60. The thus obtained aromatic containing base oil (lubricating oil base oil) can be used as base oil (a). The base oil (a) may be a mixture of two or more kinds of aromatic containing base oils (lubricating base oils) obtained as described above.

The base oil (a) thus obtained has a total aromatic content of preferably 30% by mass or more, and more preferably 30 to 60% by mass. The base oil (a) preferably has a base oil (a1) of from 200 to 1500 N, more preferably from 250 to 600 N and / or a base oil (a2) of from 600 to 1200 N, more preferably from 300 to 450 N, And / or a base oil (a2) of 700 to 1000N.

The distillation distillation fraction for obtaining an aromatic-containing base oil of 500 N may contain a large amount of the above-mentioned eight kinds of specific aromatic compounds (PAH), and it is also possible to obtain two or more types of aromatic- It tends to be difficult to do. Therefore, it is preferable to obtain an aromatic-containing base oil by using the base oil (a1) of 300 to 450 N and / or the base oil (a2) of 700 to 1000 N.

The method for producing an aromatic containing base oil according to the present embodiment is characterized in that after the second solvent extraction step at least one selected from the second extract and the second raffinate is used to obtain an aromatic containing base oil having a total aromatic content of 30 mass% And may have a base oil preparation process.

In the base oil preparation step, at least one selected from the second extract and the second raffinate is used to obtain an aromatic containing base oil having a total aromatic content of 30 mass% or more. The second raffinate was subjected to a refining treatment including a dewaxing treatment to obtain a refined oil (deaerating oil) having a pour point of -5 DEG C or lower, an aniline point of 90 DEG C or higher, a viscosity index of 90 or higher, and a flash point of 250 DEG C or higher, This may be an aromatic-containing base oil. As the refining treatment, it is preferable to carry out the dewaxing treatment and the hydrogenation finishing. Thus, an aromatic-containing base oil having a total aromatic content of 30 mass% or more can be easily obtained. The refined oil obtained by applying the above purification treatment can be suitably used as a lubricating oil base oil, a rubber compounding oil or a base thereof.

For example, when a purified oil having a viscosity of 200 to 1500 N is obtained from the second raffinate, the first and second solvent extraction steps are carried out using the reduced-pressure distillate fraction corresponding to this viscosity as the raw material, A second extract having a kinetic viscosity of preferably 200 mm 2 / s or more, more preferably 250 mm 2 / s or more, further preferably 5000 mm 2 / s or less, particularly preferably 2000 mm 2 / s or less can be obtained .

By the above process, an aromatic-containing base oil (hereinafter referred to as "aromatic-containing base oil") having a total aromatic content of 30 mass% or more from the second raffinate and / or its refined oil and / Containing base oil (hereinafter referred to as " aromatic-containing base oil b ") having a mass ratio of 30 mass% or more.

In the base oil preparation step, the oil is properly separated from the second raffinate and the second extract by distillation, and then a part of the second raffinate and a part of the second extract are treated as base oil (a), base oil (b ). The second raffinate and the second extract obtained in the second solvent extraction step may be used as the base oil (a) and the base oil (b) as they are without performing the base oil preparation step.

It is preferable to obtain the base oil (a) and base oil (b) having the desired properties as co-products by properly selecting the reduced-pressure distillation oil as the raw material in accordance with the desired base oil (a) and base oil (b). For example, when a base oil of 300 N or more and less than 600 N is obtained as the base oil (a), the above-described first and second solvent extraction processes and, in some cases, (B) having a kinematic viscosity at 40 DEG C of not less than 200 mm < 2 > / s and not more than 500 mm < 2 > / s, 350 mm < 2 > / s, more preferably 250 to 300 mm < 2 > / s.

Further, for example, when a base oil of 600 to 1200 N is obtained as the base oil (a), it is preferable to use the reduced-pressure distillate fraction corresponding to the oil fraction as the raw material and perform the above first and second solvent extraction processes, The base oil (b) has a kinematic viscosity at 40 DEG C of 500 to 5000 mm < 2 > / s, preferably 800 to 2000 mm < 2 > / s, More preferably 900 to 1500 mm < 2 > / s.

The base oil (a) of the present embodiment may be obtained by subjecting the second raffinate to a refining treatment including a dewaxing, hydrogenation, and the like as described above. The base oil (a) (lubricating base oil) thus obtained has a total aromatic content of 30 mass% or more, preferably 30 to 60 mass%. The base oil (a) can be obtained as a lubricating oil base preferably at 200 to 1500 N, more preferably at least 250 N and also at less than 600 N or 600 to 1200 N, more preferably 300 to 450 N or 700 to 1000 N.

From the viewpoint of reducing the contents of the above eight kinds of specific aromatic compounds (PAH) and obtaining base oil (a) and base oil (b) having a high flash point with different viscosities, base oil (a) To 1000N is particularly preferable.

When the base oil (a) is 600 to 1,200 N, preferably 700 to 1000 N, it is preferable that the base oil (a) further has the following characteristics in addition to the above specific properties.

- Kinematic viscosity at 40 캜: 120 to 250 mm 2 / s, preferably 150 to 200 mm 2 / s.

10% point by gas chromatography distillation: 450 to 520 占 폚, preferably 460 to 500 占 폚.

90% point by gas chromatography distillation: 540 to 600 占 폚, preferably 560 to 590 占 폚.

30% by mass or more, preferably 35 to 60% by mass, more preferably 40 to 50% by mass, of all aromatic components (ASTM D 2549).

According to this embodiment, base oils (a) and base oils (b) having a specific aromatic compound (PAH) content of not more than a predetermined amount can be obtained. In the present specification, "specific aromatic compound (PAH)" means the eight specific aromatic compounds (PAH) listed below. The base oil (a) and the base oil (b) of the present embodiment are characterized in that the content of the benzo (a) pyrene (BaP) in 1) is 1 mass ppm or less and 8 kinds of the specific aromatic compounds (PAH ) Can be set to 10 mass ppm or less.

1) benzo (a) pyrene (BaP)

2) benzo (e) pyrene (BeP)

3) Benzo (a) Anthracene (BaA)

4) Chrysene (CHR)

5) benzo (b) fluoransen (BbFA)

6) Benzo (j) Fluorans (BjFA)

7) benzo (k) fluoransen (BkFA)

8) dibenzo (a, h) anthracene (DBAhA)

These specific aromatic compounds (PAH) can generally be quantitatively analyzed by GC-MS analysis after preparing a sample to which an internal standard substance is added after separating and concentrating the target component.

The base oil (a) and base oil (b) are suitable as lubricating base oils, rubber compound oils or base materials thereof. The base oil (a) is sufficiently reduced in the content of the specific aromatic compound (PAH), and is also suitable as a lubricant base oil since the flash point is 250 ° C or higher and the pour point is -5 ° C or lower. Further, since the total aromatic content is 30 mass% or more and the glass transition point is -30 占 폚 or less, it can be used as a petroleum-based process oil or an extender oil or a base thereof.

Since the base oil (b) is sufficiently reduced in the content of the specific aromatic compound (PAH) and has a flash point of 250 ° C or higher, a total aromatic content of 30 mass% or higher and a glass transition point of -30 ° C or lower, Can be used as extender oil or as a base therefor.

By using a base oil (a), a base oil (b) or a mixture thereof, for example, a glass transition temperature of -55 to -30 캜 and a kinematic viscosity (100 캜) of 20 to 50 mm 2 / Based process oil or extender oil particularly suitable for compounding in rubber. Tires produced by blending these petroleum-based process oils or extender oils with diene rubbers can achieve both low fuel consumption and gripability, and can improve heat aging resistance and wear resistance.

As described above, according to the production method of the present embodiment, it is possible to obtain an aromatic-containing base oil having a high flash point, a low glass transition point, a high total aromatic content and a sufficiently reduced content of a carcinogenic substance at a high yield . In addition, it is particularly useful in industry because it is possible to simultaneously produce a plurality of kinds of aromatic-containing base oils having different properties with respect to a lubricating oil base oil, a petroleum-based process oil, or an extender oil or a base material thereof, and having different viscosities.

The base oil (a) preferably has the following characteristics.

Pour point: preferably -5 ° C or lower, more preferably -10 ° C or lower, and still more preferably -20 ° C or higher.

Glass transition temperature: preferably -30 占 폚 or lower, more preferably -40 占 폚 or lower, further preferably -50 占 폚 or lower, preferably -60 占 폚 or higher, more preferably -100 占 폚 or higher -80 DEG C or higher, particularly preferably -70 DEG C or higher.

Aniline point: preferably 70 占 폚 or higher, more preferably 90 占 폚 or higher, further preferably 105 占 폚 or higher, preferably 120 占 폚 or lower.

The viscosity index is preferably 90 or more, more preferably 95 or more, preferably 120 or less, more preferably 105 or less.

Flash point: preferably 250 占 폚 or higher, preferably 310 占 폚 or lower.

The base oil composition according to ASTM D 3238:% C _P is preferably 60 to 70%, C _N is preferably 20 to 30%, C _A is preferably 5 to 10%.

ㆍ Benzo (a) Pyrene content: preferably 1 mass ppm or less.

The total content of the specific aromatic compound (PAH): preferably 10 mass ppm or less.

As the base oil of base oil (a1) of 300 N or more and less than 600 N, preferably 300 to 450 N, it is preferable that the base oil has the following characteristics besides the above properties.

- Kinematic viscosity at 40 캜: preferably 60 to 120 mm 2 / s, more preferably 65 to 90 mm 2 / s, even more preferably 70 to 80 mm 2 / s.

10% by GC distillation, preferably 400 to 460 deg. C, more preferably 430 to 450 deg.

90% point by GC distillation: preferably 500-540 占 폚, more preferably 510-530 占 폚.

- Total aromatic content (ASTM D 2549): preferably 30% by mass or more, more preferably 30 to 50% by mass.

The value of the gas chromatographic distillation in this specification is a value measured in accordance with ASTM D 2887.

It is preferable that the base oil (a2) of 600 to 1200 N, preferably 700 to 1000 N, has the following characteristics in addition to the above-mentioned properties.

- Kinematic viscosity at 40 캜: preferably 120 to 250 mm 2 / s, more preferably 150 to 200 mm 2 / s.

10% point by GC distillation: preferably 450 to 520 占 폚, more preferably 460 to 500 占 폚.

90% point by GC distillation: preferably 540 to 600 占 폚, more preferably 560 to 590 占 폚.

The total aromatic content (ASTM D 2549) is preferably at least 30 mass%, more preferably from 35 to 60 mass%, still more preferably from 40 to 50 mass%.

As the base oil (b), there can be used an aromatic-containing base oil which is a second extract or its refined oil obtained by performing the above-described first and second solvent extraction steps. The base oil (b) may be a mixture of two or more kinds of the second extract obtained as described above or its refined oil.

(B1) having a kinematic viscosity at 40 占 폚 of less than 500 mm2 / s and a glass transition point of from -60 to -40 占 폚 and / or a kinematic viscosity at 40 占 폚 of 500 mm2 / , And a base oil (b2) having a glass transition point of -50 to -30 占 폚.

As the base oil (b1), it is preferable that the base oil (b1) has the following properties besides the above-mentioned properties.

A kinetic viscosity at 40 캜: preferably 200 mm 2 / s to 500 mm 2 / s, more preferably 400 mm 2 / s or less, further preferably 350 mm 2 / s or less, particularly preferably 300 mm 2 / .

Glass transition point: preferably -60 to -40 占 폚, more preferably -55 to -48 占 폚.

Pour Point: preferably 0 to 30 占 폚, more preferably 15 占 폚 or more, further preferably 20 占 폚 or more.

The difference between the pour point and the glass transition point (pour point-glass transition point): preferably 60 ° C or more, more preferably 65 ° C or more, further preferably 70 ° C or more, preferably 100 ° C or less, Below 80 ℃.

The total aromatic content is not less than 50% by mass, preferably not less than 60% by mass, more preferably not less than 70% by mass, further preferably not less than 80% by mass, preferably not more than 90% by mass.

As the base oil (b2), it is preferable that the base oil (b2) has the following properties besides the above-mentioned properties.

The kinetic viscosity at 40 占 폚 is preferably 500 mm2 / s or more, more preferably 800 mm2 / s or more, still more preferably 1000 mm2 / s or more, preferably 5000 mm2 / s or less, Mm 2 / s or less, more preferably 1500 mm 2 / s or less.

Glass transition point: preferably -50 to -30 占 폚, more preferably -45 to -35 占 폚.

The total aromatic content is not less than 50% by mass, preferably not less than 60% by mass, more preferably not less than 70% by mass, further preferably not less than 80% by mass, preferably not more than 90% by mass.

When the aromatic-containing base oil of 200 to 1500 N is obtained as the base oil (a) by the above-described first and second solvent extraction processes, by using the reduced-pressure distillation oil fraction corresponding to this oil fraction as a raw material, It is possible to obtain a kinematic viscosity at 40 캜 of preferably 200 mm 2 / s or higher, preferably 250 mm 2 / s or higher, preferably 5000 mm 2 / s or lower, more preferably 2000 mm 2 / s or lower. Further, the base oil (a) and the base oil (b) may be those obtained by appropriately separating the desired oil by distillation. In this case, the viscosity of the reduced-pressure distillation oil as a raw material is not particularly limited.

However, it is preferable to obtain the desired base oil (a) and the desired base oil (b) as the co-product, so that the decompressed distillate fraction suitable for the characteristics of the base oil (a) and base oil (b) It is preferable to use it as a raw material.

For example, in the case of obtaining an aromatic-containing base oil of 250 N or more and less than 600 N as the base oil (a1), the reduced-pressure distillate fraction corresponding to this oil fraction is used as a raw material. Then, the base oil (a1) having an kinematic viscosity of not less than 250 N but less than 600 N is obtained by the first and second solvent extraction steps, and the base oil (b1) (aromatic-containing base oil) of less than 250 g / s, preferably 250 to 350 mm2 / s, more preferably 250 to 300 mm2 / s.

Further, for example, in the case of obtaining a lubricating base oil of 600 to 1200 N as the base oil (a2), the reduced-pressure distillate fraction corresponding to this oil fraction is used as a raw material. The first and second solvent extraction steps are carried out to obtain an aromatic base oil having a base oil (a2) of 600 to 1,200 N and a base oil (b2) having a kinematic viscosity at 40 DEG C of 500 to 5000 mm < (Aromatic containing base oil) of 800 to 2000 mm < 2 > / s, more preferably 900 to 1500 mm < 2 > / s. In this method, it is preferable to carry out a batch treatment to obtain a desired base oil (a) and base oil (b).

In the compounding step, the base oil (a) and the base oil (b) obtained as described above are compounded at a predetermined ratio to prepare a rubber compounding oil. For example, the base oil (a) is blended in a proportion of 95 mass% or less (not including 0) and the base oil (b) in a proportion of 5 mass% or more, based on the rubber compounding flow rate. Thus, a rubber blend oil containing the base oil (a) and the base oil (b) can be obtained.

Further, the rubber compounding oil may be prepared by the base oil (b) alone without carrying out the above-described compounding step. However, from the viewpoint of obtaining a rubber blend oil having an appropriate kinematic viscosity (kinematic viscosity at 100 ° C of 10 to 70 mm 2 / s, preferably 15 to 50 mm 2 / s, more preferably 20 to 32 mm 2 / s) The mixing ratio of the base oil (a) is preferably 10 to 50% by mass, more preferably 10 to 50% by mass, based on the rubber compounded oil, in view of obtaining a rubber compounding oil having a difference between a pour point and a glass transition point of 50 deg. Is 20 to 40% by mass. From the same viewpoint, the blending ratio of the base oil (b) is preferably 90 to 50 mass%, and more preferably 80 to 60 mass%.

The base oil (a) preferably contains the base oil (a2), and the base oil (b) preferably contains the base oil (a2) in view of obtaining a rubber compounding oil having a difference of a pour point and a glass transition point of 50 deg. C or higher and a glass transition point of- , And the base oil (b1) is preferable in that the difference between the pour point and the glass transition point is particularly large, for example, 60 DEG C or more. The base oil (b) preferably contains the base oil (b1) and the base oil (b2) in order to increase the yield of the rubber compounding oil having the appropriate kinematic viscosity. In this respect, the content ratios of the base oil (a), base oil (a2), base oil (b1) and base oil (b2) are preferably 10 to 40 mass%, 5 to 35 mass%, and 85 to 25 mass %, More preferably 20 to 30 mass%, 20 to 30 mass%, and 60 to 40 mass%.

Further, the rubber compounding oil of the present embodiment can be compounded with a base material other than the base oil (a) and the base oil (b) so far as the effect of the present invention is not impaired.

Although the preferred embodiments of the present invention have been described above, the present invention is not limited to these embodiments at all.

Example

The present invention will be described in detail with reference to the following Examples and Reference Examples. However, the present invention is not limited to the following examples.

(Example 1)

The atmospheric distillation residue of the crude oil was distillated under reduced pressure using a conventional vacuum distillation apparatus to collect fuel equivalent oil, oil equivalent of 150N equivalent or less, oil equivalent of 350N, and oil equivalent of 900N. The aliquot equivalent to 350 N taken out was treated by a polar solvent extracting apparatus as shown in Fig. Concretely, the first solvent extraction step of introducing the oil equivalent equivalent to 350 N into the first extraction column 30 having the column bottom temperature lower than the column top temperature and bringing the polar solvent (furfural) and the equivalent of 350 N into contact with each other. By this first solvent extraction step, the oil equivalent equivalent to 350 N is mixed with the mixture of the first raffinate and the polar solvent obtained from the top portion of the first extraction tower 30 and the mixture of the first extract and the polar solvent ≪ / RTI > Thereafter, the polar solvent was recovered by a classification tower (not shown) to obtain a first raffinate and a first extract from the mixture.

Subsequently, the first raffinate was introduced into the second extraction column 40 having the column bottom temperature lower than the column top temperature, and a second solvent extraction process was performed to bring the first raffinate into contact with a polar solvent (furfural). By this second solvent extraction step, the first raffinate was separated into a mixture of the second raffinate and the polar solvent obtained from the overhead portion and a mixture of the second extract and the polar solvent obtained from the bottom portion. Thereafter, the polar solvent was recovered by a classification tower (not shown) to obtain a second extract and a second raffinate from the mixture.

The second raffinate had a total aromatic content of 30 mass% or more as measured according to ASTM D 2549. The second extract had a density of 0.94 g / cm 3 or more at 15 캜, and a total aromatic content of 30% by mass or more measured according to ASTM D 2549.

Table 1 shows the production conditions and yields of the first solvent extraction step and the second solvent extraction step.

The second raffinate was subjected to purification treatment by MEK dewaxing and hydrogenation treatment so as to have a pour point of -10 占 폚 or lower to obtain an aromatic containing base oil (lubricating base oil) having a total aromatic content of 30 mass% or more. This was used as base oil (A1). Further, the second extract was made of base oil (B1) and base oil (B3). Table 2 shows properties of base oil A1, base oil B1 and base oil B3. Further, the second extract was not subjected to purification treatment.

The total content of benzo (a) pyrene and eight kinds of specific aromatic compounds (PAH) was measured as follows. First, 1 g of each of the aromatic containing base oils was dissolved in hexane in a 50 ml flask to prepare a 2 mass% sample solution. This sample solution was loaded on a 5 mass% aqueous silica gel, washed with hexane, and eluted with 1 vol% acetone / hexane solution. After the eluate was concentrated, a sample to which an internal standard substance was added was prepared and identified and quantified by a general gas chromatograph mass spectrometer (GC-MS).

(Example 2)

The atmospheric distillation residue of the crude oil was distillated under reduced pressure using a conventional vacuum distillation apparatus to collect fuel equivalent oil, oil equivalent of 150N equivalent or less, oil equivalent of 350N, and oil equivalent of 900N. Except that the oil equivalent equivalent to 900 N was introduced into the first extraction column 30 instead of the equivalent of 350 N and the production conditions of the first and second solvent extraction processes were changed as shown in Table 3, To thereby prepare first and second raffinates, and first and second extractions. Further, the preparation was carried out plural times under the same conditions to obtain a plurality of lots of articles of manufacture. Table 3 shows the production conditions and yields of the first solvent extraction step and the second solvent extraction step.

The second raffinate in Example 2 also had a total aromatic content of at least 30 mass% measured according to ASTM D 2549. The second extract had a density of 0.94 g / cm 3 or more at 15 ° C and a total aromatic content of 30% by mass or more measured according to ASTM D 2549.

Two kinds of second raffinates having different production lots were subjected to purification treatment by MEK dewaxing and hydrogenation finishing treatment so as to have a pour point of -10 占 폚 or lower to obtain two kinds of aromatic containing base oils having a total aromatic content of 30 mass% Oil base oil). This was used as base oil A2 and base oil A3. Further, the second extract obtained in the second solvent extraction step together with the second raffinate used for producing the base oil (A2) was referred to as base oil (B2). Further, the second extract obtained in the second solvent extraction step together with the second raffinate used for producing the base oil (A3) was referred to as base oil (B4). Table 4 shows properties of base oil A2, base oil A3, base oil B2 and base oil B4.

From Table 1 and Table 3, it can be seen that, in Examples 1 and 2, the total yield of the second raffinate and the second extract, which are useful as the rubber blend oil or its base, 74 to 75% by volume (yield of useful ingredient). Thus, it was confirmed that a lubricating base oil (aromatic containing base oil) useful as a rubber blend oil or its base material can be produced at a high yield.

From Table 2 and Table 4, it can be seen that the base oil A1, the base oil A2, the base oil A3, the base oil B1, the base oil B2, the base oil B3 and the base oil B4 ) Had a total aromatic content of 30 mass% or more and a flash point of 250 deg. C or more. That is, in the present embodiment, a plurality of aromatic-containing base oils having different properties and having different properties can be produced by using a plurality of reduced-pressure distillation oils having different viscosities.

The base oil A1, the base oil A2, the base oil A3, the base oil B1, the base oil B2, the base oil B3 and the base oil B4 can be prepared from benzo (a) The total content of the specific aromatic compound (PAH) of the present invention was sufficiently reduced.

The difference between the pour point and the glass transition point of the base oil (B1) and the base oil (B2) was 50 DEG C or more. Particularly, the base oil (B1) had a characteristic that the difference was 70 DEG C or more. In other words, it was confirmed that both the base oil (B1) and the base oil (B2) had low glass transition points despite the high pour point.

The base oil (B1), base oil (B2), base oil (B3) and base oil (B4) of Examples 1 and 2 had a high aromatic hydrocarbon content (C _A ) of 20 to 35 mass% T _g ), it is possible to improve the tensile strength and abrasion resistance by blending in the rubber composition.

(Example 3)

The rubber blend oils of Examples 3-1 to 3-4 were prepared by blending the above base oils A1, base oils A2, base oils B1, and base oils B2 in the compounding ratios shown in Table 5. The properties of the respective rubber compounding ingredients are summarized in Table 5.

As shown in Table 5, all of the rubber blend oils of Examples 3-1, 3-2, 3-3 and 3-4 had a high total flash point of the aromatic component and a high toxicity of carcinogenic harmful substances . The difference between the pour point and the glass transition point was 45 ° C or more. Particularly, the rubber blend oils of Examples 3-1 and 3-2 are characterized in that the difference between the pour point and the glass transition point is 60 ° C or more, the total aromatic content by ASTM D 2549 or ASTM D 2007 is 50% by mass or more, Had a glass transition point of -45 캜 or less despite the fact that it was 15 캜 or higher.

The rubber blend oils of Examples 3-1 to 3-4 had a% C _A of 20 to 35 according to ASTM D 3238, a glass transition temperature (T _g ) of -55 to -30 캜, a kinematic viscosity (100 캜 ) Is 20 to 50 mm 2 / s, and is a petroleum-based process oil substantially free of a specific aromatic compound (PAH), and is used for processing extender oil or diene rubber used in the production process of diene rubber It is clear that both the low fuel consumption and the gripability can be achieved and the excellent effect of improving the heat aging resistance and the abrasion resistance can be obtained.

(Reference Example 1)

The atmospheric distillation residue of the crude oil was distillation under reduced pressure using a conventional vacuum distillation apparatus to collect a fuel equivalent fraction, an oil fraction equivalent to 150 N or less, an oil fraction equivalent to 250 N, and an oil fraction equivalent thereto (equivalent to 500 N). The 500N equivalent oil fraction collected is introduced into an extraction column having a column bottom temperature lower than the column top temperature to increase the raffinate yield and the aromatic fraction of the obtained lubricant base oil is 30 mass% or more and the content of the specific aromatic compound (PAH) is 10 mass ppm (Furfural) in the presence of a solvent. By this solvent extraction step, the oil equivalent of 500 N was separated into the first raffinate and the first extract. Production conditions and yields of the solvent extraction process are shown in Table 6.

The first raffinate thus obtained was subjected to purification treatment by MEK dewaxing and hydrogenation finishing treatment so that the pour point became -10 캜 or lower. Thereby, two types of aromatic-containing base oils (lubricating base oils) having a total aromatic content of 30 mass% or more with different production lots were obtained. This was used as base oil (E1) and base oil (E2). In addition, the exhaust was used as the base oil (F). Table 7 shows properties of the base oil (E1), base oil (E2) and base oil (F).

As shown in Table 6, in this Reference Example, the yield of the first raffinate based on the raw material introduced into the extraction tower was 60% by volume, and the yield of the first extract was 40% by volume. Further, as shown in Table 7, the total content of specific aromatic compounds (PAH) which are carcinogenic to the aromatic containing base oil (F) was more than 10 mass ppm. This aromatic containing base oil (F) is not suitable for use as a rubber compounding oil in this state, and even when it is blended with other lubricating base oils, the compounding ratio thereof can not usually be 50 mass% or more .

(Reference Example 2)

The deasphalted oil of the reduced pressure distillation residue of the crude residue of the atmospheric distillation residue of crude oil was separated by raffinate and extractions by the solvent extraction process as in Reference Example 1. The extract had a kinematic viscosity at 100 ° C of 95 mm 2 / s, a total aromatic content of 69 mass% by ASTM D 2549, a pour point of 12.5 ° C, a glass transition point of -29.7 ° C, Glass transition point) was 42.2 占 폚.

This extract and the base oil (E1) of Reference Example 1 were compounded in a mass ratio of 80:20 to prepare a rubber compounding oil. The pour point of the rubber compounding oil was 0 ° C, the glass transition point was -44.5 ° C, and the difference between the pour point and the glass transition point was 44.5 ° C.

(Reference Example 3)

A solvent extraction step was carried out in the same manner as in Reference Example 1 except that the oil equivalent of 250 N was fed into the extraction tower instead of the oil equivalent of 500 N to obtain raffinate and extract. Then, with respect to the raffinate, purification treatment by MEK dewaxing and hydrofinishing treatment was carried out so that the pour point became -10 ° C or lower to obtain an aromatic containing base oil. This was used as base oil (G). Base oil (g) had a flash point of less than 250 ° C. That is, in this reference example, only one kind of aromatic-containing base oil having a flash point of 250 ° C or higher (500N base oil) could be obtained from the whole amount of reduced-pressure distillate oil (equivalent to 250N oil).

According to the present invention, it is possible to provide a rubber blend oil having a high flash point and a low glass transition point while sufficiently reducing the content of a specific polycyclic aromatic compound while maintaining a high aromatic content, and a process for producing such rubber blended oils. Further, according to the present invention, the raffinate and extract obtained by the polar solvent extraction method using the reduced-pressure distillate oil as a raw material have high flash point, low glass transition point, high total aromatic content, It is possible to provide a sufficiently reduced aromatic containing base oil. It is also possible to provide a process for producing an aromatic-containing base oil capable of producing such an aromatic base oil at a high yield.

30 ... The first extraction tower, 40 ... The second extraction tower, 50 ... Scraper, 60 ... Hydrogenation finishing apparatus.

Claims (10)

A total aromatic content of 57 to 90 mass% according to ASTM D 2007 or ASTM D 2549, a flash point of 250 to 350 占 폚, a difference between a pour point and a glass transition point of 45 占 폚 or more,
The content of benzo (a) pyrene is 1 mass ppm or less, and
Wherein the total content of the specific aromatic compounds in the following 1) to 8) is 10 mass ppm or less.
1) benzo (a) pyrene (BaP)
2) benzo (e) pyrene (BeP)
3) Benzo (a) Anthracene (BaA)
4) Chrysene (CHR)
5) benzo (b) fluoransen (BbFA)
6) Benzo (j) Fluorans (BjFA)
7) benzo (k) fluoransen (BkFA)
8) dibenzo (a, h) anthracene (DBAhA) The process according to claim 1, comprising raffinate or a refined oil obtained by separating the reduced-pressure distillate fraction of the crude oil from the solvent extraction process, and further comprising a kinematic viscosity at 40 DEG C of 60 to 600 mm2 / s, 70 to 120 ℃, an aromatic containing from 400 to 500 ℃ 10% by GC distillation point, 90% point of 500 to 600 ℃, the% C _a by the ASTM D 3238 3 to 20, a glass transition point of -100 to -30 ℃ Base oils (a), and
Wherein the anhydrous distillation residue of the atmospheric distillation residue is extracted in a solvent extraction step and contains the extractant or the refined oil thereof and has a kinematic viscosity at 40 DEG C of not less than ²⁰⁰ mm < ² > / s and not more than 2000 mm < Containing base oil (b) among the aromatic-containing base oils (b) having a density of 0.94 g / cm 3 or more at 15 ° C and a total aromatic content of 30 to 90 mass% according to ASTM D 2549,
Wherein the content of the aromatic containing base oil (a) is 95 mass% or less and the content of the aromatic containing base oil (b) is 5 mass% or more. 3. The method according to claim 2,
In a first extraction column in which the column bottom temperature is 30 to 90 ° C and the column top temperature is higher than the column bottom temperature, the reduced-pressure distillate fraction and the polar solvent are brought into contact with each other to obtain a first raffinate and a first solvent extraction The process,
Wherein the first raffinate and the polar solvent are brought into contact with each other in a second extraction tower having a column bottom temperature and a column top temperature higher by at least 10 ° C than the first extraction column to obtain a second raffinate and a second extract Extraction process,
Wherein the aromatic containing base oil (b) is the second extract or the refined oil thereof. A raffinate or a refined oil obtained by separating the reduced-pressure distillation residue of the crude oil from the atmospheric distillation residue in a solvent extraction step, and further having a kinematic viscosity at 40 ° C of 60 to 600 mm 2 / s, an aniline point of 70 to 120 ° C, a GC Containing base oil (a) having a 10% point by distillation of 400 to 500 ° C, a 90% point of 500 to 600 ° C, a% C _A of 3 to 20 according to ASTM D 3238 and a glass transition point of -100 to -30 ° C, and
And an aniline point of 40 to 90 占 퐉 and a kinematic viscosity at 40 占 폚 of less than 2000 mm2 / s and an aniline point of 40 to 90 占 퐉, Containing base oil (b) having a density of 0.94 g / cm 3 or more at 15 ° C and a total aromatic content of 30 to 90% by mass according to ASTM D 2549,
(A) a pyrene content of not more than 1 mass ppm, a content of benzo (a) pyrene of not more than 1 mass ppm, And the content of the specific aromatic compound in the following 1) to 8) is 10 mass ppm or less, and the content of the aromatic containing base oil (a) is more than 0 mass% and 95 mass% Is not less than 5 mass% and less than 100 mass%.
1) benzo (a) pyrene (BaP)
2) benzo (e) pyrene (BeP)
3) Benzo (a) Anthracene (BaA)
4) Chrysene (CHR)
5) benzo (b) fluoransen (BbFA)
6) Benzo (j) Fluorans (BjFA)
7) benzo (k) fluoransen (BkFA)
8) dibenzo (a, h) anthracene (DBAhA) Distilled oil of the atmospheric distillation residue of the crude oil and the polar solvent are brought into contact with each other in the first extraction column having a column bottom temperature of 50 to 70 ° C and a column top temperature of 80 to 100 ° C to obtain a first raffinate and a first extract A second solvent extraction step
Wherein the first raffinate and the polar solvent are brought into contact with each other in a second extraction column having a column top temperature and a column top temperature higher by 10 ° C or more than the first extraction column and a density of 0.94 g / Lt; 3 > or more and a total aromatic content of 30 mass% or more,
Containing at least a part of the second extract, the second raffinate or the refined oil thereof, wherein the total aromatic content is 30 mass% or more. 6. The process of claim 5, wherein after the second solvent extraction step, the second raffinate is subjected to a refining treatment including a dewaxing treatment to obtain the refined oil,
Wherein the purified oil contains the pour point of -20 to -5 占 폚, the aniline point of 90 to 120 占 폚, the viscosity index of 90 to 120, and the flash point of 250 to 310 占 폚. 6. The method of claim 5, further comprising at least a portion of the second extract,
A kinematic viscosity at 40 DEG C of not less than 500 mm < 2 > / s, a flash point of not less than 250 DEG C, a pour point of not more than 30 DEG C, an aniline point of not more than 90 DEG C and a glass transition point of -60 to -40 DEG C, Wherein the glass transition point difference is 50 DEG C or more. 6. The process for producing an aromatic containing base oil according to claim 5, wherein the content of the benzo (a) pyrene is 1 mass ppm or less, and the total content of the specific aromatic compounds in the following 1) to 8) is 10 mass ppm or less.
1) benzo (a) pyrene (BaP)
2) benzo (e) pyrene (BeP)
3) Benzo (a) Anthracene (BaA)
4) Chrysene (CHR)
5) benzo (b) fluoransen (BbFA)
6) Benzo (j) Fluorans (BjFA)
7) benzo (k) fluoransen (BkFA)
8) dibenzo (a, h) anthracene (DBAhA) An aromatic containing base oil obtained by the production method according to any one of claims 5 to 8. A rubber compounding oil containing the aromatic-containing base oil according to claim 9.

Images