KR20120004408A - Rubber compounding oil and method for producing same - Google Patents

Abstract

It contains an extract (A) and a lubricant base oil (B), and the extract (A) has an aniline point of 40 to 90 ° C, 25 to 45% C _A according to ASTM D3238, 5 to 20% C _{N according} to ASTM D3238, nitrogen content 0.01 mass% or more, a pour point of +30 degrees C or less, content of benzo (a) pyrene is 1 mass ppm or less, the sum total content of a specific aromatic compound is 10 mass ppm or less, and the kinematic viscosity in 40 degreeC is 650 mm <2> / s The above lubricating oil base oil (B) has a pour point of −10 ° C. or less, an aniline point of 70 ° C. or more,% C _A of ASTM D3238 3 to 20,% C _N of 15 to 35, and nitrogen content of 0.01 mass% or less. The rubber compounding oil whose 90% point in GC distillation is 500 degreeC or more, the flash point is 250 degreeC or more, content of benzo (a) pyrene is 1 mass ppm or less, and the sum total content of a specific aromatic compound is 10 mass ppm or less.

Description

Rubber compounding oil and method for producing same

The present invention relates to a rubber compounding oil and a method for producing the same.

Since high aromatic mineral oil has high affinity with a rubber component, and is excellent in workability, softening property, and economical efficiency of a rubber composition, it is used for manufacture of rubber compositions, such as natural rubber and synthetic rubber. For example, synthetic rubber such as SBR is blended with extender oil (extender oil) at the time of its synthesis, and processed oil in rubber-processed products such as tires in order to improve the processability and quality of the rubber-processed product. (Process oil) is mix | blended (for example, patent document 1).

In Patent Literature 1, the aromatic hydrocarbon content (C _A ) is 20 to 35% by weight, the glass transition temperature (T _g ) is -55 to -30 ° C, the kinematic viscosity (100 ° C) is 20 to 50 mm 2 / s, and is also polycyclic. It is proposed to use petroleum process oil whose aromatic component amount (PCA) is 3 weight% or less in petroleum process oil. When the rubber obtained by blending this petroleum process oil with a diene rubber is used for a tire, both low fuel consumption and grip characteristics can be achieved, and heat aging resistance and heat abrasion resistance can be improved.

As rubber compounding oil, highly aromatic base oils, such as a vacuum distillation residue, deasphalted oil, deasphalted oil, or the solvent extraction extract of lubricating oil, are known (for example, patent document 2). However, when such a high aromatic base oil is used as a high flash point from the standpoint of safety or to be outside the scope of the dangerous oil fourth petroleum oil under Japanese law, the pour point becomes high and the pour point becomes high, thereby reducing workability during storage, transportation and handling. Here, in order to lower the pour point, it is also proposed to dewax the high aromatic base oil, but the manufacturing process is complicated and the economical efficiency is significantly deteriorated. For this reason, the rubber compounding oil which does not require a complicated manufacturing process and has a high viscosity, a high flash point, and a low pour point is calculated | required.

On the other hand, in Europe, a regulation that a certain amount of DMSO extract or a specific carcinogenic polycyclic aromatic compound should not be used for the production of tires or tire parts has been applied since 2010, and rubber formulations conforming to these regulations are applied. Oil is required.

Japanese Unexamined Patent Publication No. 2004-155959 : Japanese Patent Publication No. 3658155

The present invention has been made in view of the above circumstances, and provides a rubber compounding oil having a high flash point and a high aromaticity, sufficiently reducing the content of a specific carcinogenic polycyclic aromatic compound, and having a low pour point and excellent economic efficiency, and a method for producing the same. For the purpose of

As a result of intensive studies on the description of the rubber compounding oil, the present inventors have found a specific carcinogenic polycyclic aromatic compound having a high viscosity, a high flash point and a high aromaticity by using a specific extract and a specific lubricant base oil. Specific aromatic compound ”) was sufficiently reduced, and it was found that a rubber compounded oil having a low flow point excellent in economic efficiency was obtained, thus completing the present invention.

That is, the present invention is a rubber compounding oil containing the extract (A) and the lubricating oil base oil (B), the extract (A) has an aniline point of 40 to 90 ℃,% C _A according to ASTM D3238 is 25 to 45 and% C _N in the 5 to 20, jilsobun is 0.01 mass% or more and a pour point + 30 ℃ or less, benzo (a) the content of the pyrene is 1 mass ppm or less, a total content of the specific aromatic compound 10 mass ppm or less, and 40 ℃ in dynamic viscosity is 650㎟ / s and above, the lubricating oil base oil (B) has a pour point below -10 ℃, aniline point above 70 ℃, according to ASTM D3238% C _a of 3 to 20 and% C _N of 15 to 35, Nitrogen content is 0.01 mass% or less, 90% point in GC distillation is 500 degreeC or more, flash point is 250 degreeC or more, content of benzo (a) pyrene is 1 mass ppm or less, and the sum total content of a specific aromatic compound is 10 mass ppm or less And rubber compounding oil.

According to the said invention, by containing a specific extract (A) and lubricating oil base oil (B), it can be set as the rubber compounding oil which has a high flash point and high aromaticity, the content of a specific aromatic compound is fully reduced, and its pour point is low. . Moreover, since it is possible to manufacture without making a manufacturing process complicated, it can be made excellent also in economic efficiency.

The rubber compounding oil of the present invention has a flash point of 250 ° C. or more, an aniline point of 90 ° C. or less, a kinematic viscosity at 40 ° C. of 200 mm 2 / s or more, a pour point of + 30 ° C. or less, and a benzo (a) pyrene (BaP) It is preferable that content is 1 mass ppm or less and the sum total of content of said specific aromatic compound is 10 mass ppm or less. In addition, the rubber compounding oil of the present invention, in order to improve the low fuel consumption, grip properties and heat aging resistance when the diene rubber composition described in Patent Document 1, in particular,% C _A is 20 to 35, The glass transition temperature (T _g ) is -55 to -30 ° C, the kinematic viscosity (100 ° C) is 20 to 50 mm 2 / s, and the content of benzo (a) pyrene (BaP) is 1 ppm by mass or less, and the specific aromatics described above. It is preferable that the sum total of content of a compound is 10 mass ppm or less, and it is more preferable that a pour point is +20 degrees C or less, especially +15 degrees C or less.

In the rubber compounding oil of the present invention, the extract (A) is extracted by contacting the deasphalted oil obtained by deasphalting the vacuum distillation residue of the atmospheric distillation residue of crude oil in one or two stages with a polar solvent. It is preferred to be a tract.

In the rubber compounding oil of the present invention, the extract (A) contains an extract obtained by a two-step polar solvent extraction step, and the extract has a bottom temperature of 30 to 90 ° C and a top temperature of the bottom temperature. Raffinate and the polar solvent obtained by contacting the vacuum distillation fraction of the crude oil atmospheric distillation residue with the polar solvent in the first extraction column higher than the first extraction column, respectively, It is obtained by making it contact in an extraction column, and it is preferable that the density in 15 degreeC of an extract is 0.94 g / cm <3> or more, and the total aromatic content by ASTM D2549 is 30 mass% or more.

In the rubber compounding oil of the present invention, the lubricant base oil (B) is obtained by the dewaxed oil (c) of the first raffinate and / or the polar solvent extraction step of the two stages obtained by the one-step polar solvent extraction step. The dewaxed oil (d) of the second raffinate is contained, and the dewaxed oil (c) has a bottom bottom temperature of 30 to 90 ° C. and a top bottom temperature of the first extraction column having a higher top temperature than that of the atmospheric distillation residue of crude oil. The first raffinate obtained by contacting the distillate under reduced pressure with a polar solvent was subjected to a purification treatment including a dewaxing step. The dewaxed oil (d) has a bottom temperature and a top temperature of 10 ° C., respectively, than the first extraction column. In the above-mentioned second extraction tower, it is preferable that the second raffinate obtained by contacting the first raffinate and the polar solvent is subjected to a purification treatment including a dewaxing step.

In this invention, an aniline point of 40 to 90 ℃, according to ASTM D3238% C _A of 25 to 45 and% C _N is 5 to 25, jilsobun is 0.01 mass% or more and a pour point + 30 ℃ or less, benzo (a Extract (A) having a content of pyrene of 1 mass ppm or less, a total content of a specific aromatic compound of 10 mass ppm or less, and a kinematic viscosity at 40 ° C. of 650 mm 2 / s or more, and a pour point of -10 ° C. or less, and aniline point above 70 ℃, according to ASTM D3238% C _a of 3 to 20 and% C _N of 15 to 35, jilsobun is 0.01 mass% or less, more than 500 ℃ 90% point of the GC distillation, flash point of more than 250 ℃, The manufacturing method of rubber compounding oil which has the process of mix | blending the lubricating oil base oil (B) whose content of benzo (a) pyrene is 1 mass ppm or less and the sum total content of a specific aromatic compound is 10 mass ppm or less is provided.

According to the production method of the present invention, by mixing the specific extract (A) and the lubricating oil base oil (B), a rubber compounding oil having a high flash point and a high aromaticity, the content of the specific aromatic compound is sufficiently reduced, and the fluid viscosity is low. It can manufacture. Moreover, since the manufacturing method of this invention can manufacture without making a manufacturing process complicated, it is excellent also in economy.

According to the present invention, it is possible to provide a rubber compounding oil having a high flash point and a high aromaticity, sufficiently reducing the content of a specific aromatic compound, and having a low pour point and excellent economic efficiency, and a method for producing the same.

BRIEF DESCRIPTION OF THE DRAWINGS It is a process schematic diagram which shows an example of the manufacturing method of the base material used for the rubber compounding oil of this invention.
2 is a process schematic diagram showing another example of the method for producing a base material used in the rubber compounding oil of the present invention.
3 is a process schematic diagram showing still another example of the method for producing a base material used in the rubber compounding oil of the present invention.

EMBODIMENT OF THE INVENTION Hereinafter, preferred embodiment of this invention is described with reference to drawings. In addition, the same number is attached | subjected to the same or equivalent thing, and the overlapping description is abbreviate | omitted as needed.

The rubber compounding oil of this embodiment is the extract (A) (henceforth simply called "(A) component") which has a specific characteristic, and the lubricating oil base oil (B) which has a specific characteristic (hereinafter, simply It is a rubber compounding oil containing "(B) component."

Component (A) is less than an aniline point of 40 to 90 ℃, according to ASTM D3238% C _A is 25 to 45,% C _N is from 5 to 20, jilsobun more than 0.01 wt%, pour point + 30 ℃, benzo (a) 1 mass ppm or less of pyrene, the sum total of a specific aromatic compound is 10 mass ppm or less, and is an extract whose dynamic viscosity in 40 degreeC is 650 mm <2> / s or more.

As long as the extract which is (A) component is satisfied, the extract obtained at the polar solvent extraction process may be used as it is, and the extract may be subjected to the purification treatment. Here, as a purification process, dewaxing, hydrocracking, hydrorefining, distillation, etc. are mentioned. Moreover, as (A) component, it is preferable to use the extract obtained by the polar solvent extraction process as it is, without adding a refinement | purification process from a viewpoint of making it more suitable property for manufacturing cost and a rubber compounding oil. As this reason, the rubber compounding oil which is excellent in low temperature performance is obtained, the tendency for aromaticity to become low when hydrocracking does not need to be dewaxed, and the manufacturing method becomes complicated when refining is added.

The aniline point of (A) component is 40-90 degreeC, Preferably it is 45-70 degreeC, More preferably, it is 50-65 degreeC. If the aniline point is in the above range, even if it contains a lubricating oil base oil having a high aniline point as the component (B), it is easy to manufacture a rubber compounding oil having a good aniline point in order to maintain excellent properties of the rubber composition and excellent compatibility with rubber. Lose. In addition, the aniline point in this specification means the aniline point measured based on JISK2256-1985.

(A) is a composition of the components,% C _A of 25 to 45, preferably 30 to 40 ℃ and,% C _N is from 5 to 20, preferably 6 to 12. In addition,% C _P is, but be determined by the% C _A,% C _N, and preferably from 35 to 70, more preferably from 48 to 64. If the composition of the component (A) is within the above range, a rubber compounding oil having a composition suitable for maintaining the properties of the rubber composition is excellent in compatibility with rubber even if the component (B) contains a highly paraffinic lubricant oil. It becomes easy to manufacture. Further, referred to here% C _P,% C _N and% C _A are each method in accordance with ASTM D3238-85 a percentage of the total number of carbon atoms of the paraffin carbon number of which is determined by the (ndM ring analysis), naphthenic carbons Means a percentage with respect to the total carbon number, and a percentage with respect to the total carbon number of the aromatic carbon number.

The nitrogen content of (A) component is 0.01 mass% or more, Preferably it is 0.05 mass% or more, More preferably, it is 0.1 mass% or more, Especially preferably, it is 0.15 mass% or more. The higher the nitrogen content of the component (A), the lower the nitrogen content of the by-product raffinate by polar solvent extraction and the higher the refining efficiency of the lubricating oil base oil. Therefore, it is economical to use the component (A) having a high nitrogen content as the rubber compounding oil. It is preferable at the point of view. In addition, nitrogen content in this invention means nitrogen content by the chemiluminescence method measured based on JISK2609.

The pour point of (A) component is +30 degrees C or less, Preferably it is +5-+25 degreeC, From a viewpoint of further lowering the pour point of a rubber compounding oil, More preferably, it is +5-+20 degreeC, Especially preferably, +7.5 to + 15 ° C.

In order to contain the component (B) mentioned later, the rubber compounding oil of this embodiment has a sufficiently low pour point, even when it contains the crude (A) component with a high pour point. In addition, a pour point in this specification means the pour point measured based on JISK2269.

As for (A) component, content of the eight types of aromatic compounds (together, it calls it a "specific aromatic compound") listed below is fully reduced.

1) Benzo (a) pyrene (BaP)

2) benzo (e) pyrene (BeP)

3) benzo (a) anthracene (BaA)

4) Chrysene (CHR)

5) benzo (b) fluoranthene (BbFA)

6) benzo (j) fluoranthene (BjFA)

7) benzo (k) fluoranthene (BkFA)

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

Here, benzo (a) pyrene in this specification means benzo (a) pyrene (BaP) of said 1), and a specific aromatic compound means aromatic compound (PAH) of said 1) -8). .

Content of benzo (a) pyrene (BaP) of 1) in (A) component is 1 mass ppm or less, and the sum total of content of the specific aromatic compound of 1) -8) is 10 mass ppm or less. As a result, a rubber compounding oil having higher safety without carcinogenicity can be obtained. Moreover, after separating and concentrating a target component, this specific aromatic compound can prepare the sample which added the internal standard substance, and can quantitatively analyze by GC-MS analysis.

The kinematic viscosity at 40 ° C of the component (A) is 650 mm 2 / s or more, preferably 800 mm 2 / s or more, more preferably 2000 mm 2 / s or more, still more preferably 5000 mm 2 / s or more, Preferably it is 20000mm <2> / s or less, More preferably, it is 10000mm <2> / s or less.

When the kinematic viscosity at 40 ° C of the component (A) is less than 650 mm 2 / s, even if the component (B) is contained, there is a tendency that a sufficiently low pour point is not obtained. When the kinematic viscosity at 40 ° C of the component (A) is set to 700 mm 2 / s or more, preferably 800 mm 2 / s or more, the pour point of the rubber compounding oil may be made to be 15 ° C. or less. In this case, the pour point of the component (A) is preferably +5 to + 20 ° C, more preferably +7.5 to + 15 ° C.

In this embodiment, the kinematic viscosity at 40 ° C is 650 mm 2 / s or more, and preferably, the rubber compound having a low flow point by containing the component (A) and the component (B) having a pour point of +5 to + 20 ° C. I can do it. Moreover, when the kinematic viscosity of (A) component exceeds 20000mm <2> / s, the kinematic viscosity suitable as a rubber compounding oil (kinematic viscosity in 100 degreeC is 10-70mm <2> / s, Preferably it is 15-50mm <2> / s, Especially Preferably, the rubber compounding oil having 20 to 32 mm 2 / s) tends to be difficult to be obtained. In addition, dynamic viscosity in each temperature said in this specification means dynamic viscosity in each temperature measured based on JISK2283.

The asphaltene component of the component (A) is preferably 3% by mass or less, more preferably 1% by mass or less, still more preferably 0.5% by mass or less, and particularly preferably 0.1% by mass or less. In addition, the asphaltene powder mentioned in this specification means the asphaltene powder measured based on IP-143.

The flash point of the component (A) is preferably 250 ° C or more, more preferably from the viewpoint of the safety of the rubber compounding oil from the viewpoint of safety, or from being outside the scope of the dangerous petroleum fourth petroleum oil according to the Japanese Fire Law according to safety. 270 degreeC or more, More preferably, it is 290 degreeC or more, Especially preferably, it is 300 degreeC or more. In addition, the flash point as used in this specification means the flash point by Cleveland opening type (COC) measured based on JISK2265.

The total aromatic content of the component (A) is preferably 50% by mass or more, more preferably 55% by mass or more, even more preferably 60% by mass or more, particularly preferably 65% by mass or more. On the other hand, the total aromatic content of (A) component becomes like this. Preferably it is 90 mass% or less, More preferably, it is 80 mass% or less, More preferably, it is 75 mass% or less. When the total aromatic content of the component (B) is less than 50% by mass, it is difficult to obtain a highly aromatic rubber compounding oil. When the total aromatic content exceeds 90% by mass, the yield in the polar solvent extraction step is lowered. This tends to increase the manufacturing cost. In addition, the total aromatic content as used in this specification means content of the aromatic fraction (aromatics fraction) measured based on ASTMD2549.

(B) component contained rubber compounding oil of the present embodiment, the pour point is -10 ℃ or less, aniline point is from 3 to 20% C _A by more than 70 ℃, ndM analysis,% C _N of 15 to 35, the jilsobun It is a lubricating oil base oil whose 0.01 mass% or less, 90% point in GC distillation is 500 degreeC or more, a flash point 250 degreeC or more, 1 mass ppm or less of benzo (a) pyrene, and the sum total of a specific aromatic compound is 10 mass ppm or less.

Pour point of (B) component is -10 degrees C or less, and may be less than -20 degreeC. However, from the viewpoint of keeping the pour point of the rubber compounding oil low and reducing the production cost, the temperature is preferably -10 to -20 ° C. By using the component (B) having a pour point of −10 ° C. or lower, a rubber compounded oil having a low pour point can be obtained.

The aniline point of (B) component is 70 degreeC or more, Preferably it is 90 degreeC or more, More preferably, it is 100 degreeC or more. On the other hand, since it becomes easy to manufacture the rubber compounding oil which has the compatibility with rubber and is suitable for maintaining the characteristic of a rubber composition, it is 120 degrees C or less.

(B) is a composition of the components,% C _A is 3 to 20, preferably 5 to 10, and,% C _N is from 15 to 35, preferably from 20 to 30. In addition,% C _P is determined according to% C _A ,% C _N , but is preferably 45 to 82, more preferably 60 to 75, still more preferably 65 to 70. By using the component (B) whose composition is the said range, it becomes easy to manufacture the rubber compounding oil which is excellent in compatibility with rubber | gum, and has a composition suitable for maintaining the characteristic of a rubber composition.

The nitrogen content of (B) component is 0.01 mass% or less, Preferably it is 0.008 mass% or less. In addition, although the nitrogen content of (B) component may be less than 0.001 mass%, from a viewpoint of the manufacturing cost reduction of the rubber compounding oil by using the lubricating oil base oil with low refinement degree, Preferably it is 0.002 mass% or more, More preferably, it is 0.003 mass More than%

The flash point of (B) component is 250 degreeC or more from a viewpoint of making the flash point of rubber compounding oil 250 degreeC or more and out of the dangerous goods 4th petroleum, Preferably it is 255 degreeC or more. Moreover, since the flash point of (A) component is also high, the flash point of (B) component does not need to be made higher than necessary, Preferably it is 290 degrees C or less, More preferably, it is 280 degrees C or less.

The 90% point in GC distillation of (B) component is 500 degreeC or more, Preferably it is 500-600 degreeC. In this embodiment, it is preferable to use the thing of 510-550 degreeC in 90% points in GC distillation of (B) component. On the other hand, as another embodiment, it is preferable to use what is 90 to 550 degreeC in 90% point in GC distillation of (B) component. There is no restriction | limiting in particular in 10C point in GC distillation of (B) component, From a viewpoint of safety, or from the viewpoint of making it the target of dangerous goods fourth petroleum of Japan's fire law by setting it as 250 degreeC or more, Preferably it is 400-510 degreeC, More preferably, it is 440-500 degreeC. As one form, what is 440-470 degreeC, and as another form is what is 450-500 degreeC can be used.

Content of benzo (a) pyrene (BaP) of said 1) in (B) component is 1 mass ppm or less, and the sum total of content of said specific aromatic compound is 10 mass ppm or less. Thereby, rubber compounding oil with low carcinogenicity and high stability can be obtained.

The kinematic viscosity at 40 ° C. of the component (B) is preferably 50 to 500 mm 2 / s, more preferably 60 to 300 mm 2 / s, still more preferably 70 to 200 mm 2 / s. In this embodiment, when using (A) component whose kinematic viscosity in 40 degreeC is 2000 mm <2> / s or more, in order to obtain the rubber compounding oil of a suitable kinematic viscosity, the kinematic viscosity in 40 degreeC of (B) component is obtained. The component (B) is preferably 50 to 150 mm 2 / s, more preferably 80 to 120 mm 2 / s. Moreover, when using the (A) component whose kinematic viscosity in 40 degreeC is less than 2000 mm <2> / s as another embodiment, in order to obtain the rubber compounding oil of a suitable kinematic viscosity, in 40 degreeC of (B) component, The kinematic viscosity is preferably 50 to 500 mm 2 / s, more preferably 60 to 80 mm 2 / s and / or 120 to 250 mm 2 / s of component (B).

The total aromatic content of the component (B) is preferably 20% by mass or more, more preferably 30% by mass or more, and still more preferably 35% by mass or more. On the other hand, the total aromatic content of the component (B) is preferably 50% by mass or less, and more preferably 45% by mass or less. When the total aromatic content of the component (B) is less than 20% by mass, it is difficult to obtain a rubber compounding oil having a high aromaticity. On the other hand, when total aromatic content exceeds 50 mass%, the oxidation stability at the time of using it as lubricating oil base oil of (B) component will fall remarkably, and it will become difficult to combine with lubricating oil base oil and rubber compounding oil use, and a petroleum refining process The economy of the whole tends to be lowered.

The rubber compounding oil of this embodiment can be obtained by mix | blending said (A) component and (B) component. In addition, the rubber compounding oil of this embodiment can mix | blend base materials other than (A) component and base materials other than (B) component, unless the effect of this invention is impaired remarkably.

In order to have the affinity with a rubber, softening property, high flash point, safety, and handling, and the low fuel consumption, grip property, and heat aging resistance at the time of manufacturing a rubber composition, the rubber compounding oil of this embodiment is It is preferable to have the following various characteristics.

Density at 15 ° C: usually 0.9 g / cm 3 to 1.0 g / cm 3, preferably 0.94 g / cm 3 or more, more preferably 0.945 g / cm 3 or more, preferably 0.98 g / cm 3 or less, more preferably Is 0.96 g / cm 3 or less.

Flash point: Usually 250-350 degreeC, Preferably it is 260 degreeC or more, More preferably, it is 280 degreeC or more, Preferably it is 320 degrees C or less, More preferably, it is 310 degrees C or less.

Dynamic viscosity in 40 degreeC: Usually 200-3000 mm <2> / s, Preferably it is 300 mm <2> / s or more, More preferably, 400 mm <2> / s, More preferably, 500 mm <2> / s or more, Preferably 2000 mm <2> / s or less, More preferably, it is 1000 mm <2> / s or less, More preferably, it is 800 mm <2> / s or less.

Kinematic viscosity at 100 ° C: usually 10 to 100 mm 2 / s, preferably 15 mm 2 / s or more, more preferably 20 mm 2 / s or more, preferably 60 mm 2 / s or less, more preferably 50 mm 2 / s, More preferably, it is 32 mm <2> / s or less.

Aniline point: Usually 50-100 degreeC, Preferably it is 60 degreeC or more, More preferably, it is 65 degreeC or more, More preferably, it is 70 degreeC or more, Preferably it is 90 degrees C or less, More preferably, it is 85 degrees C or less.

Nitrogen content: Usually 0.01-0.2 mass%, Preferably it is 0.03 mass% or more, More preferably, it is 0.05 mass% or more, Preferably it is 0.15 mass% or less, More preferably, it is 0.1 mass% or less.

% C _N : Usually 5-30, Preferably it is 10 or more, More preferably, it is 14 or more, Preferably it is 25 or less, More preferably, it is 20 or less.

% C _A : Usually 10-40, Preferably it is 17 or more, More preferably, it is 20 or more, Preferably it is 35 or less, More preferably, it is 30 or less, More preferably, it is 25 or less.

% C _P : 30 to 85, preferably 40 or more, more preferably 50 or more, preferably 73 or less, and more preferably 66 or less.

Total aromatic component (ASTM D2549): Usually 30-90 mass%, Preferably it is 40 mass% or more, More preferably, it is 50 mass% or more, Preferably it is 80 mass% or less, More preferably, it is 70 mass% or less. .

Saturated content by ASTM D2007 (clay gel method): 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

Aromatic component by ASTM D2007 (claygel method): usually 40 to 90 mass%, preferably 50 mass% or more, more preferably 55 mass% or more, still more preferably 57 mass% or more, particularly preferably 60 It is mass% or more, Preferably it is 80 mass% or less, More preferably, it is 70 mass% or less.

Polar compound powder by ASTM D2007 (claygel method): Usually 1-20 mass%, Preferably it is 2 mass% or more, More preferably, it is 5 mass% or more, Preferably it is 15 mass% or less, More preferably, 12 It is mass% or less, More preferably, it is 10 mass% or less.

Saturation content / polar compound content ratio by ASTM D2007 (clay gel method): Usually 0.25-50, Preferably it is 1 or more, More preferably, it is 2.5 or more, More preferably, it is 3 or more, Preferably it is 20 or less, More preferably, it is 10 or less, More preferably, it is five or less.

Content of benzo (a) pyrene (BaP): It is 1 mass ppm or less.

The sum total of content of the said specific aromatic compound: It is 10 mass ppm or less.

Pour point: -10 to +30, Preferably it is -5 degreeC or more, Preferably it is +15 degreeC or less, More preferably, it is +5 degreeC or less, More preferably, it is 0 degrees C or less.

Glass transition point (T _g ): -60 to -10 ° C, preferably -55 ° C or more, preferably -30 ° C or less, more preferably -40 ° C or less, still more preferably -45 ° C or less, Especially preferably, it is -48 degrees C or less.

"Glass transition point (T _g )" of the aromatic-containing base oil in this specification means the calorie | heat amount in a glass transition area | region measured when heated up at a constant temperature increase rate (10 degree-C / min) by DSC (differential scanning calorimeter). The glass transition point obtained from the change peak. The initial temperature is usually about 30 to 50 ° C. or lower than the expected glass transition point, and after holding for a certain time at the initial temperature, the temperature is started. In this embodiment, it can measure on the following conditions specifically.

Apparatus: Thermal analysis system DSC Q100 made by T-A Instruments

Initial temperature: -90 ℃, hold for 10 minutes

Temperature rise rate: 10 ℃ / min

Termination temperature: 50 ℃, hold for 10 minutes

In addition, the method of calculating a glass transition point from a calorie change peak can be determined by the method of JISK7121.

The rubber compounding oil of this embodiment can be obtained by mix | blending (A) component and (B) component. There is no restriction | limiting in particular in the content rate of (A) component and (B) component, For example, the content rate of (A) component is 5-95 mass% on the basis of the rubber compounding oil whole quantity, Preferably it is 40-90 mass% to be. However, since an actual pour point is lower than the pour point expected from the pour point of (A) component and (B) component which are base materials, it is preferably 55-85 mass%. Moreover, from a viewpoint of setting it as the rubber compounding oil which has an appropriate viscosity and a lower pour point, Preferably it is 40-75 mass%, More preferably, it is 55-75 mass%.

Similarly, the compounding ratio of (B) component is 5-95 mass% on the basis of the rubber compounding oil whole quantity, Preferably it is 10-60 mass%. The content rate is 5-95 mass% on the basis of the rubber compounding oil whole quantity, Preferably it is 40-90 mass%. However, since the actual pour point of rubber compounding oil is lower than the pour point anticipated from the pour point of (A) component and (B) component which are base materials, the content rate of (B) component becomes like this. Preferably it is 15-45 mass%. . Moreover, from a viewpoint of setting it as the rubber compounding oil which has an appropriate viscosity and a lower pour point, Preferably it is 25-60 mass%, More preferably, it is 25-45 mass%.

The rubber compounding oil of this embodiment can be obtained by mix | blending (A) component and (B) component in said ratio. Next, the manufacturing method of (A) component and (B) component which are base materials of a rubber compounding oil is demonstrated.

[Method for Producing (A) Component]

The method for producing the component (A) is not particularly limited as long as the properties of the component (A) described above are satisfied. The method of deasphalting and extracting by contacting the obtained deasphalted oil with a polar solvent is mentioned.

Hereinafter, with reference to drawings, two manufacturing methods (a "first form" and a "second form" for convenience) of (A) component are explained in full detail.

(First form)

1: is a process schematic diagram which shows an example of the manufacturing method of (A) component. In the first aspect, first, a deasphalting step of deasphalting the vacuum distillation residue oil is performed. The deasphalting process may be one step or two or more steps. However, two stages of raffinate having different kinematic viscosities useful as base oils for lubricating oil and two or more extracts having different kinematic viscosities suitable as rubber compounding oils can be obtained, respectively. It is preferable to use the above deasphalting process. On the other hand, it is preferable that the deasphalting process is two steps or less from a viewpoint of avoiding the complicated process. Hereinafter, the method of performing a deasphalting process in two steps of a 1st deasphalting process and a 2nd deasphalting process is demonstrated.

(First deasphalting process)

In the first deasphalting process, the vacuum distillation residue of the crude oil at atmospheric pressure distillation residue and the deasphalting solvent are counter-currently contacted in the first deasphalting tower 10 to separate the first deasphalting oil and the first deasphalting oil. 1 It is a process of obtaining deasphalted oil and a 1st containing asphalt oil. The deasphalted solvent is circulated and used as appropriate by using a recovery tower (not shown) provided on the downstream side of the first deasphalted tower 10 or the like.

The deasphalted solvent is supplied from the piping 14 to the 1st deasphalted top 10. On the other hand, the vacuum distillation residue oil is supplied from the piping 12 to the 1st deasphalting tower 10. FIG. And the 1st deasphalted oil from the piping 16 and the 1st containing asphalt oil from the piping 18 are obtained.

As a deasphalting solvent, nonpolar light hydrocarbons, such as propane and butane, Preferably propane is used. The deasphalted condition is kinematic viscosity at 100 ° C. of the first deasphalted oil, preferably 10 to 35 mm 2 / s, more preferably 15 to 30 mm 2 / s, still more preferably 18 to 28 mm 2 / s. . The deasphalted temperature can be adjusted by changing the top temperature and / or bottom temperature of the 1st deasphalted tower 10. As shown in FIG. Deasphalting conditions of a 1st deasphalting process can be performed as follows, for example.

Solvent ratio: As a volume ratio based on the vacuum distillation residue oil, Preferably it is 1-6, More preferably, it is 1.5-4, More preferably, it is 2-4.

Top temperature of the first deasphalted tower 10: Preferably it is 60-120 degreeC, More preferably, it is 80-100 degreeC, More preferably, it is 85-95 degreeC.

Top bottom temperature of the 1st deasphalted tower 10: Preferably it is 50-100 degreeC, More preferably, it is 60-90 degreeC, More preferably, it is 70-85 degreeC.

Yield of 1st deasphalted oil: Based on the vacuum distillation residue oil, Preferably it is 1-30 volume%, More preferably, it is 2-20 volume%, More preferably, it is 3-15 volume%.

The 1st deasphalted oil obtained in this way is used for the 1st polar solvent extraction process mentioned later, and is isolate | separated into a 1st raffinate and a 1st extract. In addition, you may use the 1st containing asphalt oil (residual oil which is not extracted in a deasphalting solvent: oil containing much asphaltene powder) as an asphalt raw material as it is. In addition, it is preferable that the 1st asphalt containing oil uses the 2nd containing asphalt oil obtained by isolate | separating 2nd deasphalted oil by the 2nd deasphalting process mentioned later as an asphalt raw material.

(2nd deasphalting process)

In the second deasphalting process, the first deasphalted oil and the deasphalted solvent are countercurrently contacted in the second deasphalted tower 20 to be separated into the second deasphalted oil and the second deasphalted oil, and the second deasphalted oil is removed. It is a process of obtaining asphalt oil and a 2nd asphalt oil. The deasphalted solvent is appropriately recovered by using a recovery tower (not shown) or the like provided on the downstream side of the second deasphalted tower 20, and circulated and used.

The deasphalted solvent is supplied from the pipe 24 to the second deasphalted tower 20. On the other hand, the 1st asphalt oil is supplied from the piping 18 to the 2nd deasphalted tower 20. As shown in FIG. Then, the second deasphalted oil is obtained from the pipe 26, and the second asphalted oil is obtained from the pipe 28.

As the deasphalting solvent, nonpolar light hydrocarbons such as propane and butane, preferably propane, are used as in the first deasphalting step. Although the deasphalting solvent used for a 2nd deasphalting process may be the same as or different from a 1st deasphalting process, it is more preferable to use the same deasphalting solvent from a viewpoint of simplifying a process.

The deasphalting conditions in the second deasphalting step are not particularly limited as long as they are different from the deasphalting conditions in the first deasphalting step. As for the deasphalting conditions in a 2nd deasphalting process, the kinematic viscosity in 100 degreeC of 2nd deasphalting oil is 30-60 mm <2> / s, Preferably it is 35-50 mm <2> / s, More preferably, It is preferable to adjust so that it may be 36-45 mm <2> / s. As such conditions, the following conditions are mentioned, for example.

Solvent ratio: As a volume ratio based on a 1st asphalt containing oil, it is 1-10, Preferably it is 4-8, More preferably, it is 5-7.

Top temperature of the 2nd deasphalted tower 20: 50-110 degreeC, Preferably it is 60-80 degreeC. It is preferable that it is 10-30 degreeC, More preferably, it is 15-25 degreeC lower than the top temperature of a 1st deasphalted tower.

Top bottom temperature of the 2nd deasphalted tower 20: 40-80 degreeC, Preferably it is 50-60 degreeC.

Yield of second deasphalted oil: 15 to 50% by volume, preferably 20 to 45% by volume, more preferably 25 to 40% by volume, based on the first asphalt-containing asphalt oil which is a raw material of the second deasphalted oil process. to be.

The solvent ratio in the second deasphalting step is preferably 1.5 to 10 times the solvent ratio in the first deasphalting step, more preferably 2 to 5 times, and even more preferably 2.5 to 4 times. Do.

The top temperature in the second deasphalting step is preferably 10 to 30 ° C lower than the top temperature in the first deasphalting step, and more preferably 15 to 25 ° C lower. The bottom temperature in the second deasphalting step is preferably 10 to 30 ° C lower than the bottom temperature in the first deasphalting step, and more preferably 15 to 25 ° C lower.

(1st polar solvent extraction process (1))

In the first polar solvent extraction step (1), the first deasphalted oil and the polar solvent are countercurrently contacted in the first extraction column 30 to separate the first deasphalted oil into the first raffinate and the first extract, It is a process of obtaining a 1st raffinate and a 1st extract. The polar solvent is appropriately recovered using a recovery tower (not shown) or the like provided on the downstream side of the first extraction tower 30, and circulated for use. Examples of the polar solvent include polar solvents such as furfural, phenol, cresol, sulfolane, N-methylpyrrolidone, dimethyl sulfoxide, formylmorpholine, and glycol solvents. In this embodiment, general lubricant base oils are used. It is preferable to use furfural from the point that the solvent extraction facility can be converted.

The polar solvent is supplied from the pipe 34 to the first extraction tower 30. Meanwhile, the first deasphalted oil passes through the pipe 16 and is supplied to the first extraction tower 30. Then, the first raffinate is obtained from the pipe 36 and the first extract is obtained from the pipe 38.

There is no restriction | limiting in particular in extraction conditions, For example, extraction conditions are made so that the kinematic viscosity in 100 degreeC of a 1st extract may become 30-70mm <2> / s, More preferably, it is 40-60mm <2> / s. I can adjust it. Extraction conditions of a 1st polar solvent extraction process can be performed as follows, for example.

Solvent ratio: As a volume ratio based on 1st deasphalted oil, Preferably it is 1-5, More preferably, it is 2-4, More preferably, it is 2.5-3.5.

Top temperature in the first extraction column 30: Preferably it is 100-150 degreeC, More preferably, it is 120-140 degreeC, More preferably, it is 126-136 degreeC.

Top bottom temperature in the first extraction column 30: Preferably it is 60-130 degreeC, More preferably, it is 80-125 degreeC, More preferably, it is 86-120 degreeC.

Yield of the first extract: Preferably it is 15-50 volume%, More preferably, it is 20-40 volume%, More preferably, it is 25-33 volume% based on 1st deasphalted oil.

(2nd polar solvent extraction process (1))

In the second polar solvent extraction process, the second deasphalted oil and the polar solvent are countercurrently contacted in the second extraction tower 40 to separate the second extract and the second raffinate, and the second extract and the second raffinate. To obtain. The polar solvent is circulated and used as appropriate by using a recovery tower (not shown) or the like provided on the downstream side of the second extraction tower 40. As a polar solvent, the same thing as the said 1st polar solvent extraction process (1) can be used. In addition, from the viewpoint of process simplification, it is preferable to use the same polar solvent used in the first and second polar solvent extraction steps.

The polar solvent is supplied from the pipe 44 to the second extraction tower 40. On the other hand, the second deasphalted oil passes through the pipe 26 and is supplied to the second extraction tower 40. The second raffinate is obtained from the pipe 46 and the second raffinate is obtained from the pipe 48.

There is no restriction | limiting in particular in extraction conditions, For example, the kinematic viscosity in 100 degreeC of a 2nd extract becomes like this. Preferably it is 70-150 mm <2> / s, More preferably, it is 80-120 mm <2> / s, More preferably, It is preferable to adjust so that it may be 90-100 mm <2> / s. Extraction conditions other than that can be made like the said 1st polar solvent extraction process (1). Specifically, it can be as follows.

Solvent ratio: As a volume ratio based on 2nd deasphalted oil, Preferably it is 1-5, More preferably, it is 2-4, More preferably, it is 2.5-3.5.

Top temperature of the second extraction column 40: Preferably it is 100-150 degreeC, More preferably, it is 120-140 degreeC, More preferably, it is 126-136 degreeC.

Bottom temperature of the second extraction column 40: Preferably it is 60-130 degreeC, More preferably, it is 80-125 degreeC, More preferably, it is 86-120 degreeC.

2nd extract yield: It is 15-50 volume% with respect to 2nd deasphalted oil, Preferably it is 20-40 volume%, More preferably, it is 25-33 volume%.

(A) component in this embodiment is from the 1st extract in the said 1st polar solvent extraction process (1), and / or the 2nd extract in the said 2nd polar solvent extraction process (1). Can be obtained. In addition, it is preferable that (A) component is a 2nd extract from a viewpoint of making a yield high.

(Second form)

(A) component of this embodiment can be obtained also by the manufacturing method demonstrated below other than said 1st aspect. In this 2nd aspect, the 2nd extract which is (A) component is obtained by the two-step polar solvent extraction process from the vacuum distillation fraction of the atmospheric distillation residue of crude oil.

(1st polar solvent extraction process (2))

It is a process schematic diagram which shows the 2nd aspect of the manufacturing method of (A) component. First, in the first polar solvent extraction step (2), the first extraction tower 30 having the bottom temperature of 30 to 90 ° C. and the top temperature of the bottom solvent temperature of the vacuum distillation fraction and the polar solvent of the atmospheric distillation residue oil of crude oil is higher. ) To obtain a first raffinate and a first extract.

The vacuum distillate fraction used as a raw material in the first polar solvent extraction step (2) is not particularly limited, and the component is not limited to light lubricant oil, heavy lubricant oil, heavy lubricant oil, or these. Or a distillate under reduced pressure may be used.

In order to raise the flash point of an aromatic containing base oil and to make (B) component of the appropriate viscosity range which is not too high viscosity, it is 200-1500 N, Preferably 250-1200 N, More preferably, 300-600 N and / or 600 Lubricating oil fractions of 1 to 1200 N are used.

In addition, "N" in this specification means that it is neutral oil obtained from vacuum distillation fraction, for example, if it is 300N, the viscosity in 100 degrees F (37.8 degreeC) is 300 Seybolt universal herb (SUS). Means that.

In this embodiment, atmospheric distillation of crude oil such that lubricating oil base oils of 200 to 1500 N, preferably 250 to 600 N and / or 600 to 1200 N, more preferably 300 to 450 N and / or 700 to 1000 N are obtained as component (B). It is preferable to select the vacuum distillation fraction of a residue.

In the first polar solvent extraction step (2), the vacuum distillation fraction and the polar solvent are countercurrently contacted in the first extraction column 30 to separate the first deasphalted oil into the first raffinate and the first extract, A first raffinate and a first extract are obtained. The polar solvent is circulated and used as appropriate by using a recovery tower (not shown) or the like provided on the downstream side of the first extraction tower 30. The kind of polar solvent is the same as that of the said 1st polar solvent extraction process (1).

The polar solvent is supplied from the pipe 34 to the first extraction tower 30. On the other hand, the distillation under reduced pressure is supplied to the first extraction tower 30 through the pipe 16. Then, the first raffinate is obtained from the pipe 36 and the first extract is obtained from the pipe 38.

The bottom temperature of the first extraction column 30 is 30 to 90 ° C, preferably 50 to 70 ° C, more preferably 55 to 65 ° C. The top temperature of the first extraction tower 30 is higher than the bottom temperature, preferably 10 to 50 ° C., more preferably 15 to 40 ° C., and even more preferably 25 to 35 ° C., higher. More specifically, the top temperature is preferably 60 to 120 ° C, more preferably 80 to 100 ° C, still more preferably 85 to 95 ° C.

The solvent ratio in the 1st polar solvent extraction process (2) is 0.5-3, Preferably it is 0.7-2, More preferably, it is 1-1.5. In addition, the solvent ratio used in this specification means the capacity ratio (solvent amount / raw material) of the solvent with respect to a raw material.

The yield of the 1st raffinate obtained by said extraction conditions is 50-90 volume% normally, Preferably it is 60-85 volume%, More preferably, it is 70-80 volume%. The yield of the first extract is usually 10 to 50% by volume, preferably 15 to 40% by volume, more preferably 20 to 30% by volume.

By the above extraction conditions, the specific aromatic compound can be extracted to the first extract side. For this reason, the quantity of the specific aromatic compound of the lubricating oil base oil (component (B)) obtained from the 2nd extract and the 2nd raffinate obtained at a later process can fully be reduced.

(2nd polar solvent extraction process (2))

The 2nd polar solvent extraction process (2) uses the 1st raffinate obtained in the 1st polar solvent extraction process (2) as a raw material. The first raffinate and the polar solvent are subjected to countercurrent contact in the second extraction column 41 to separate the second extract and the second raffinate, thereby obtaining the second extract and the second raffinate. A polar solvent can use the same thing as the 1st polar solvent extraction process (2). In addition, from the viewpoint of process simplification, it is preferable to use the same polar solvent used in the first and second polar solvent extraction steps.

The polar solvent is supplied from the pipe 44 to the second extraction tower 41. On the other hand, the first raffinate is supplied to the second extraction tower 41 through the pipe 36. Then, the second raffinate is obtained from the pipe 47, and the second extract is obtained from the pipe 49.

The bottom temperature of the 2nd extraction tower 41 is 10 degreeC or more higher than the top bottom temperature of the 1st extraction tower 30 in the 1st polar solvent extraction process 1, Preferably it is 10-50 degreeC higher, and more Preferably it is 15-40 degreeC high, More preferably, it is 20-30 degreeC high. More specifically, the bottom temperature of the 2nd extraction tower 41 becomes like this. Preferably it is 40-140 degreeC, More preferably, it is 60-100 degreeC, More preferably, it is 80-95 degreeC.

The top temperature of the second extraction column 41 is preferably 10 to 50 ° C, more preferably 15 to 40 ° C, still more preferably 25 to 35 ° C higher than the bottom temperature. Specifically, the top temperature of the second extraction column 41 is preferably 50 to 150 ° C, more preferably 80 to 140 ° C, still more preferably 110 to 130 ° C.

The solvent ratio in the 2nd polar solvent extraction process (2) is 1-4, Preferably it is 1.3-3.5, More preferably, it is 1.5-3.3, and the solvent ratio in the 1st polar solvent extraction process (2) It is preferable to make it 1.5 times or more.

By setting it as said extraction condition, the yield of a 2nd raffinate is 50-90 volume% normally, Preferably it is 60-85 volume%, More preferably, it is 70-85 volume%, The yield of a 2nd extract, It is usually 10 to 50% by volume, preferably 15 to 40% by volume, more preferably 15 to 30% by volume.

The density in 15 degreeC of the obtained 2nd extract is 0.94 g / cm <3> or more, and the total aromatic content by ASTM D2549 is 30 mass% or more. Such a second extract can be used as the component (A).

The density at 15 ° C of the second extract is preferably 0.95 to 1 g / cm 3, more preferably 0.95 to 0.98 g / cm 3. The total aromatic content of the second extract is 30% by mass or more, preferably 60% by mass or more, more preferably 80% by mass or more, preferably 90% by mass or less. In addition, all the aromatic content in this specification is measured based on ASTMD2549.

The second extract has a% C _{A as} measured by ASTM D2140, preferably 15 to 35, preferably 20 to 33, more preferably 22 to 32.

In addition, the second extract has the following properties.

Flash point: 250 degreeC or more, Preferably it is 260 degreeC or more, Preferably it is 310 degrees C or less.

Pour point: 30 degrees C or less, Preferably it is 10-30 degreeC.

Aniline point: 90 degrees C or less, Preferably it is 40-80 degreeC, More preferably, it is 50-70 degreeC.

Benzo (a) pyrene content: It is 1 mass ppm or less.

-Total content of a specific aromatic compound: It is 10 mass ppm or less.

(Method for Producing (B) Component)

There is no restriction | limiting in particular in the manufacturing method of (B) component in this embodiment. As the component (B), for example, a vacuum-reduced distillation fraction of the atmospheric distillation residue of crude oil or a deasphalted oil obtained by deasphalting the vacuum distillation residue of the atmospheric distillation residue of crude oil is extracted and treated with a polar solvent such as furfural, The obtained raffinate can be obtained by applying a purification treatment including dewaxing, hydrogenation and the like.

Moreover, although it is also possible to use hydrocracking mineral oil, hydroisomerization mineral oil, etc. as (B) component, it does not need to be especially high quality. It can be said that the use of lubricating oil base oil having a total aromatic content of 30% by mass or more, obtained under relatively mild refining conditions, is preferable from the viewpoint of improving the suitability as a rubber compounding oil and economical efficiency.

When using (A) component whose kinematic viscosity in 40 degreeC is 2000 mm <2> / s or more, in order to obtain the rubber compounding oil of suitable kinematic viscosity, as (B) component, Preferably the kinematic viscosity in 40 degreeC is 50 It is preferable to use (B) component which is -150 mm <2> / s, Preferably it is 80-120 mm <2> / s.

On the other hand, when using the (A) component whose kinematic viscosity in 40 degreeC is less than 2000mm <2> / s, in order to obtain the rubber compounding oil of suitable kinematic viscosity, Preferably kinematic viscosity in 40 degreeC is 50-500mm <2> / s, Preferably it is preferable to use 60-80 mm <2> / s and / or (B) component of 120-250 mm <2> / s.

Hereinafter, two manufacturing methods (it is called "a 1st form" and "a 2nd form" for convenience) are demonstrated in detail, referring drawings.

(First form)

(1st polar solvent extraction process (3))

3 is a process schematic diagram showing the first embodiment of the method for producing the component (B).

In the 1st polar solvent extraction process (3), the vacuum distillation fraction of the atmospheric distillation residue oil of crude oil is used as a raw material. The distillate under reduced pressure and the polar solvent are countercurrently contacted in the first extraction column 30 to separate the first extract and the first raffinate, thereby obtaining the first extract and the first raffinate. The polar solvent is appropriately recovered using a recovery tower (not shown) or the like provided on the downstream side of the first extraction tower 30, and circulated for use. The polar solvent used is the same as the manufacturing method of said (A) component.

As the distillate under reduced pressure, in order to obtain a lubricating oil base oil having a high flash point, it is preferably 200 to 800 N equivalent oil, preferably 350 to 700 N equivalent oil, and more preferably 400 to 600 N equivalent oil.

The polar solvent is supplied from the pipe 34 to the first extraction tower 30. On the other hand, the distillation under reduced pressure is supplied to the first extraction tower 30 through the pipe 16. Then, the first raffinate is obtained from the pipe 36 and the first extract is obtained from the pipe 38.

Purification treatment by the dewaxing device 50 and the hydrogenation finishing device 60 can be applied to the obtained first raffinate to obtain a lubricating oil base oil as the component (B). In addition, as a dewaxing apparatus 50 and the hydrogenation finishing apparatus 60, a normal apparatus can be used.

The bottom temperature of the 1st extraction tower 30 in the 1st polar solvent extraction process 3 is 30-90 degreeC, Preferably it is 60-80 degreeC, More preferably, it is 65-75 degreeC. On the other hand, the top temperature of the first extraction tower 30 is higher than the bottom temperature, preferably 20 to 80 ° C higher, more preferably 30 to 70 ° C higher, and even more preferably 40 to 60 ° C high. More specifically, the top temperature of the first extraction column 30 is preferably 80 to 160 ° C, more preferably 100 to 140 ° C, still more preferably 110 to 130 ° C.

The solvent ratio in the 1st polar solvent extraction process (3) is 0.5-4, Preferably it is 1-3, More preferably, it is 1.5-2.5.

By the above extraction conditions, the yield of the first raffinate obtained is usually 40 to 80% by volume, preferably 50 to 70% by volume, more preferably 55 to 65% by volume, and the yield of the first extract. Silver is usually 20 to 60% by volume, preferably 30 to 50% by volume, more preferably 35 to 45% by volume.

Since the specific aromatic compound is extracted to the 1st extract side by said extraction conditions, content of the specific aromatic compound of the lubricating oil base oil obtained from a 1st raffinate can fully be reduced.

Next, by applying purification treatment such as solvent dewaxing and hydrogenation finishing to the first raffinate, a lubricating oil base oil having a kinematic viscosity at 50 ° C of 50 to 150 mm 2 / s, preferably 80 to 120 mm 2 / s ( Component B)).

In addition, when the reduced pressure distillate fraction of 400-600 N is used as a raw material, a flash point is 250 degreeC or more, and the kinematic viscosity in 40 degreeC is 50-150 mm <2> / s, Preferably it is 80-120 mm <2> / s, GC distillation The component (B) having a 10% point by 430 to 480 ° C and a 90% point by 520 to 560 ° C can be obtained.

(Second form)

2 is a process schematic diagram showing the second embodiment of the method for producing the component (B). In this embodiment, after the second raffinate is obtained by a two-step polar solvent extraction step, the second raffinate is subjected to a purification treatment including dewaxing treatment to obtain a lubricant base oil as the component (B). .

(1st polar solvent extraction process (4))

In the 1st polar solvent extraction process (4), the vacuum distillation fraction of the atmospheric distillation residue oil of crude oil is used as a raw material. The vacuum distillation fraction and the polar solvent are countercurrently contacted in the first extraction column 30 to separate the first extract and the first raffinate, thereby obtaining the first extract and the first raffinate. The polar solvent is appropriately recovered using a recovery tower (not shown) or the like provided on the downstream side of the first extraction tower 30, and circulated for use. The kind of polar solvent is the same as that of the said 1st form.

The bottom temperature of the 1st extraction tower 30 in the 1st polar solvent extraction process 4 is 30-90 degreeC, and makes the tower temperature higher than a tower bottom temperature.

(2nd polar solvent extraction process (4))

Next, in the 2nd extraction tower 41 which has the bottom temperature and the top temperature which are 10 degreeC or more higher than the bottom temperature and the top temperature in the 1st polar solvent extraction process 4, respectively, a 1st raffinate and a polar solvent Is contacted to obtain a second raffinate and a second extract. Lubricating oil base oil which is (B) component can be obtained by adding the refinement | purification process containing the dewaxing apparatus 50 and the hydrogenation finishing apparatus 60 to this 2nd raffinate. In addition, as a dewaxing apparatus 50 and the hydrogenation finishing apparatus 60, a normal apparatus can be used.

This production method is a tablet comprising a dewaxing treatment on a second raffinate obtained by a process similar to the two-step polar solvent extraction step described in detail in the second aspect of the above-mentioned "manufacturing method of (A) component". It is the method of adding a process and obtaining the lubricating oil base oil which is (B) component. The first polar solvent extraction step 4 and the second polar solvent extraction step 4 can be performed in the same manner as the first polar solvent extraction step 2 and the second polar solvent extraction step 2.

By the above production method, it is possible to obtain a lubricant base oil (component (B)) of 200 to 1500 N, preferably 250 to 600 N and / or 600 to 1200 N, more preferably 300 to 450 N and / or 700 to 1000 N. .

In the case of using a reduced pressure distillate fraction corresponding to 300 to 400 N as a raw material, the flash point is 250 ° C or higher, and the kinematic viscosity at 40 ° C is 60 to 80 mm 2 / s, and 10% point by GC distillation is 400 to 460 ° C. , (B) component with a 90% point of 500-540 degreeC can be obtained.

In addition, when using the vacuum distillation fraction equivalent to 700N-1000N as a raw material, a flash point is 250 degreeC or more, the kinematic viscosity in 40 degreeC is 120-250mm <2> / s, and 10% point by GC distillation is 450-520 degreeC , (B) component with a 90% point of 540-600 degreeC can be obtained.

As mentioned above, although preferred embodiment of this invention was described, this invention is not limited to the said embodiment at all. For example, in the manufacturing apparatus shown in FIG. 1 used by the 1st form of the manufacturing method of said (A) component, the dewaxing provided in the downstream of the 1st extraction tower 30 and the 2nd extraction tower 40, respectively. By the apparatus 50 and the hydrogenation finishing apparatus 60, you may refine | purify 1st, 2nd raffinate, and may obtain lube base oil which is (B) component.

Example

Hereinafter, although this invention is demonstrated further more concretely based on an Example and a comparative example, this invention is not limited to a following example at all.

(Examples 1 to 3, Comparative Example 1)

[Production of (A) Component]

(A) component was manufactured using the manufacturing apparatus shown in FIG. Specifically, the vacuum distillation residue of crude oil at atmospheric pressure distillation residue and propane are brought into countercurrent contact with the first deasphalting tower 10 to depressurize the distillation residue of propane, and the first deasphalted oil and the first hammered asphalt. Oil (residue not extracted by propane) was separated (first deasphalting process).

In the 1st deasphalting process, the yield of 1st deasphalted oil (the thing which distilled propane) is 1-20 volume% with respect to the said vacuum distillation residue oil, and the kinematic viscosity in 100 degreeC of 1st deasphalted oil is 15-21. The deasphalting conditions (solvent ratio, column top temperature, and column bottom temperature) were adjusted so that it might be set to 30 mm <2> / s. The solvent ratio was adjusted in the range of 1-4, the tower top temperature of 80-100 degreeC, and the tower bottom temperature of 60-90 degreeC by the volume ratio based on the vacuum distillation residue.

Next, the first hamp asphalt oil and propane are countercurrently contacted in the second deasphalting tower 20 to propatal the first asphalt oil, and the second deasphalted oil and the second hamp asphalt oil (extracted by propane). Unoccupied residue) was separated (second deasphalting process).

In the second deasphalting step, the yield of the second deasphalting oil (propane distilled off) is 15 to 50% by volume relative to the vacuum distillation residue oil, which is a raw material in the first deasphalting step, of the second deasphalting oil. The deasphalted conditions (solvent ratio, top temperature, and bottom temperature) were adjusted so that kinematic viscosity in 100 degreeC might be 30-60 mm <2> / s. The solvent ratio was made larger than the 1st deasphalting process, and the top temperature and the bottom temperature of the 2nd deasphalting tower 20 were lower than the top temperature and the bottom temperature of the 1st deasphalting tower 10, respectively. Specifically, the solvent ratio was adjusted in the range of 60-90 degreeC and 40-80 degreeC with 4-8, top temperature, and bottom temperature in the volume ratio based on the 1st containing asphalt oil.

Table 1 describes the deasphalted conditions of the first deasphalted process and the second deasphalted process, and the yields of the deasphalted oil and the asphalt containing oil obtained.

Next, the first deasphalted oil and the second deasphalted oil are countercurrently contacted with furfural in the first extraction tower 30 and the second extraction tower 40, respectively, to thereby extract the first extract A1 and the second extract. The tract (A2) was obtained (a first polar solvent extraction step (1) and a first polar solvent extraction step (2)).

In the 1st polar solvent extraction process (1), the kinematic viscosity in 100 degreeC of a 1st extract is 30-70mm <2> / s, and the yield of a 1st extract is 15-45 volume% with respect to 1st deasphalted oil. The extraction conditions (solvent ratio, the top temperature of the first extraction tower 30 and the bottom temperature) were adjusted so that the aniline point was 90 degrees C or less, the flash point was 250 degrees C or more, and the asphaltene content was 3 mass% or less. Specifically, the solvent ratio was adjusted in a range of 2 to 4, a top temperature of 100 to 150 ° C, and a bottom temperature of 60 to 130 ° C in a volume ratio based on the first deasphalted oil.

In the 1st polar solvent extraction process (2), the kinematic viscosity in 100 degreeC of a 2nd extract is 70-150 mm <2> / s, and the yield of a 2nd extract is 15-45 volume% with respect to 2nd deasphalted oil. Extraction conditions (solvent ratio, the top temperature of the 2nd extraction tower 40, and the bottom temperature) were adjusted so that aniline point might be 90 degrees C or less, a flash point 250 degreeC or more, and asphaltene content 3 mass% or less. Specifically, the solvent ratio was adjusted in a range of 2 to 4, a top temperature of 100 to 150 ° C, and a bottom temperature of 60 to 130 ° C in a volume ratio based on the second deasphalted oil.

In Table 2, the extraction conditions of the 1st polar solvent extraction process (1) and the 1st polar solvent extraction process (2), and the yield of the 1st extract A1 and the 2nd extract A2 are described. In addition, the refinement | purification process was not added to the 1st extract A1 and the 2nd extract A2.

[Production of (B) Component]

(B) component was manufactured using the manufacturing apparatus as shown in FIG. Specifically, 500 N equivalent fraction was prepared as a vacuum distillation fraction of the atmospheric distillation residue of crude oil. This 500 N equivalent fraction was countercurrently contacted with furfural in the first extraction column 30 to obtain a first raffinate and a first extract C (first polar solvent extraction step (3)).

The bottom temperature in the 1st extraction tower 30 was 30-90 degreeC, and the top temperature was made into temperature higher than the top bottom temperature. Purification treatment such as dewaxing treatment and hydrogenation finishing treatment was added to the obtained first raffinate to obtain a lubricating oil base oil (B1). The extraction conditions of the first polar solvent extraction step (3) and the yields of the first raffinate and the first extract (C) are shown in Table 3.

First extract A1 (substrate 1) obtained in first polar solvent extraction step (1), second extract A2 (substrate 2) obtained in first polar solvent extraction step (2), first Lubricating oil base oil (B1) obtained by purifying the first extract (C) (base 3) obtained in the polar solvent extraction step (3) and the first raffinate obtained in the first polar solvent extraction step (3) ( The properties of description 4) are shown in Table 4.

As shown in Table 4, in each of the first extract A1 and the second extract A2, the content of the specific aromatic compound was less than the specific amount (10 ppm). On the other hand, in the 1st extract (C) obtained from the 1st polar solvent extraction process (3) of vacuum distillation fraction, content of the specific aromatic compound exceeded the specific amount.

The second extract (A2) and the lubricating oil base oil (B1) obtained as described above were blended in the ratios shown in Table 5 to prepare rubber compounding oils of Examples 1 to 3. In addition, the 1st extract (C) and the lubricating oil base oil (B1) were mix | blended in the ratio shown in Table 5, and the rubber compounding oil of the comparative example 1 was prepared. The properties of each rubber compounding oil are shown in Table 5.

The expected pour point in Table 5 is calculated from the pour point of (A) the second extract A2 and the pour oil of the lubricating oil base oil B1 on the premise that causticity is established.

From Table 5, the rubber compounding oil of Examples 1-3 showed the pour point at least 5 degreeC lower than the expected pour point computed from the pour point of a base material. Moreover, it was confirmed that content of the specific aromatic compound of the rubber compounding oil of Examples 1-3 is less than a specific amount. Especially, the rubber compounding oil of Example 2 had a pour point of -5 degreeC, and was 7.5 degreeC lower than the expected pour point. On the other hand, in the rubber compounding oil of the comparative example 1, content of the specific aromatic compound exceeded the specific amount.

The composition of the rubber compounding oil of Example 2 was analyzed in accordance with ASTM D2007 (clay gel method). As a result, the saturation content was 30.5 mass%, the aromatic content 61.3 mass%, the polar compound 8.2 mass%, and the saturation content / polar compound ratio 3.7. It was.

(Examples 4 and 5, Comparative Examples 2 and 3)

[Production of (A) Component]

(A) component was manufactured using the manufacturing apparatus as shown in FIG. Specifically, the vacuum distillation fraction (350 N equivalent fraction) of the atmospheric distillation residue of crude oil and furfural are counter-currently contacted in the first extraction column 30 to obtain 350 N equivalent fraction, and the first raffinate and the first extract (D ). The bottom temperature in the 1st extraction tower 30 was 30-90 degreeC (1st polar solvent extraction process (2)).

Next, the first raffinate and furfural were countercurrently contacted in the second extraction column 41 to separate the first raffinate into the second raffinate and the first extract A3 (second polar solvent extraction step). (2)). The top temperature and the bottom temperature of the second extraction tower 41 in the second polar solvent extraction step 2 are the top temperatures of the first extraction tower 30 in the first polar solvent extraction step 2 and It was 10 degreeC or more higher than top bottom temperature, respectively.

This obtained the 2nd extract (A3) whose 2nd raffinate and the density in 15 degreeC are 0.94 g / cm <3> or more and the total aromatic content measured based on ASTMD2549 is 30 mass% or more.

In Table 6, the extraction conditions of the 1st polar solvent extraction process (2) and the 2nd polar solvent extraction process (2), and the yield of each raffinate and an extract are described.

The first polar solvent extraction step (2) and the second polar solvent extraction step (2) were carried out except that the vacuum distillation fraction (900 N equivalent fraction) of the atmospheric distillation residue of crude oil was used as a raw material and the extraction conditions were slightly changed. As described above, the first polar solvent extraction step (2) and the second polar solvent extraction step (2) are performed using the manufacturing apparatus shown in FIG. 2, and the first raffinate and the first extraction column 30 are separated from the first extraction column 30. The first extract (E) has a density at the second raffinate and 15 ° C. from the second extraction column 41 at 0.94 g / cm 3 or more, and the total aromatic content measured in accordance with ASTM D2549 is 30% by mass or more. A second extract A4 was obtained.

Table 7 lists the extraction conditions of the first polar solvent extraction step (2) and the second polar solvent extraction step (2) when the 900 N equivalent fraction is used as the vacuum distillate fraction, and the yield of each raffinate and extract. do.

In the first extracts (D and E) in Tables 6 and 7, the content of the specific aromatic compound exceeded 10 mass ppm.

Next, MEK dewaxing treatment and hydrogenation finishing treatment were applied to the second raffinate in Tables 6 and 7, to obtain lube base oil (B2) and base oil (B3), respectively. Further, the obtained second extract A3 and the second extract A4 were mixed at 37.5: 62.5 (mass ratio), and the second extract A5 having a kinematic viscosity at 40 ° C. was less than 650 mm 2 / s. Obtained.

The properties of the second extracts A4 and A5 and the lubricating oil base oils B2 and B3 thus obtained are shown in Table 8.

The 2nd extract (A4) and lube base oil (B2 or B3) obtained as mentioned above were mix | blended in the ratio shown in Table 9, and the rubber compounding oil of Examples 4 and 5 was prepared. Moreover, the 2nd extract (A5) or the 1st extract (E) and (B) lubricating oil base oil (B3) were mix | blended in the ratio shown in Table 9, and the rubber compounding oil of the comparative examples 2 and 3 was prepared. The properties of each rubber compounding oil are shown in Table 9.

The expected pour point in Table 9 is computed from the pour point of (A) 2nd extract A2, the pour point of (B) lubricating oil base oil B1, and these mixture ratios on the premise that causticity holds.

From Table 9, the rubber compounding oil of Examples 4 and 5 showed the pour point at least 5 degreeC lower than the expected pour point computed from the pour point of the base material. In addition, content of the specific aromatic compound of the rubber compounding oil of Examples 4 and 5 was less than specific amount (10 ppm). On the other hand, the rubber compounding oil of the comparative example 2 showed the value higher than anticipated pour point, and the content of the specific aromatic compound of the rubber compounding oil of the comparative example 3 exceeded the specific amount.

In addition, about the rubber compounding oil of Example 1, Example 2, Example 3, and Example 4, and Example 5, glass transition point (T _g ) is measured by said method using DSC (differential scanning calorimeter). As a result, they were -44.5 degreeC, -51.3 degreeC, and -55.0 degreeC, and -52.5 degreeC, and -51.7 degreeC, respectively. That is, Examples 1-5 of rubber compounding oil, by mixing the certain X-tract and the lubricating oil base oil, referred to in the Patent Document 1,% C _A of 20 to 35 and a glass transition temperature (T _g) is -55 to -30 The viscosity and the kinematic viscosity (100 ° C.) satisfy the requirements of 20 to 50 mm 2 / s, and the sum of the contents of the specific aromatic compound (PAH) can be set to a predetermined amount or less, and the pour point is lower than the expected pour point. It became.

Therefore, the rubber compounding oils of Examples 1 to 5 are, for example, natural rubber (NR), various butadiene rubbers (BR), various styrene-butadiene copolymer rubbers (SBR), polyisoprene rubbers (IR), butyl rubbers ( When blended with a diene rubber such as BR) and any of these blended rubbers, in particular a diene rubber containing at least one styrene-butadiene copolymer rubber, both low fuel consumption and grip properties can be achieved, and heat aging resistance and abrasion resistance can be achieved. Can be improved.

Industrial availability

According to the present invention, it is possible to provide a rubber compounding oil having a high flash point and a high aromaticity, sufficiently reducing the content of a specific aromatic compound, and having a low pour point and excellent economic efficiency, and a method for producing the same.

10... First deasphalted tower, 20... Second deasphalted tower, 30... First extraction column, 40, 41... Second extraction column, 50... Dewaxing device, 60... Hydrogenation finisher.

Claims (5)

As a rubber compounding oil containing an extract (A) and a lubricating oil base oil (B),
The extract (A),
Aniline point 40 to 90 ℃,
% C _A according to ASTM D3238 is 25 to 45 and% C _N is 5 to 20,
Nitrogen content is 0.01 mass% or more,
Pour point is below +30 ℃,
1 mass ppm or less of content of benzo (a) pyrene,
The sum total content of a specific aromatic compound is 10 mass ppm or less, and the kinematic viscosity in 40 degreeC is 650 mm <2> / s or more,
The lubricating oil base oil (B),
Pour point is below -10 ℃,
Aniline point is more than 70 ℃,
% C _A according to ASTM D3238 is from 3 to 20 and% C _N is from 15 to 35,
Nitrogen content is 0.01 mass% or less,
90% point in GC distillation is 500 degreeC or more,
Flash point above 250 ℃,
1 mass ppm or less of content of benzo (a) pyrene, and
The rubber compounding oil whose total content of a specific aromatic compound is 10 mass ppm or less. The method of claim 1, wherein the extract (A) is
A rubber compounded oil, which is an extract extracted by contacting a deasphalted oil obtained by deasphalting a vacuum distillation residue of crude oil with a polar solvent by deasphalting in one or two stages. The extract (A) according to claim 1, wherein the extract (A) contains an extract obtained by a two-step polar solvent extraction process,
The extract is polarized with raffinate obtained by contacting the vacuum distillation fraction of the crude distillation residue of crude oil with a polar solvent in a first extraction tower having a bottom temperature of 30 to 90 ° C. and a top temperature higher than the bottom temperature. The solvent is obtained by contacting the bottom temperature and the top temperature in the second extraction column, each having a temperature of 10 ° C. or more higher than the first extraction column,
The rubber compounding oil whose density in 15 degreeC of the said extract is 0.94 g / cm <3> or more, and the total aromatic content by ASTM D2549 is 30 mass% or more. The dewaxed oil (c) of the first raffinate and / or the polarity of two stages according to any one of claims 1 to 3, wherein the lubricating oil base oil (B) is obtained by the polar solvent extraction process of one stage. It contains the dewaxed oil (d) of the second raffinate obtained by the solvent extraction step,
The dewaxed oil (c) is the first extraction column obtained by contacting a reduced pressure distillate of the atmospheric distillation residue of crude oil with a polar solvent in a first extraction tower having a bottom temperature of 30 to 90 ° C. and a top temperature higher than the bottom temperature. Obtained by subjecting the raffinate to a purification treatment comprising a dewaxing process,
The dewaxed oil (d) is added to the second raffinate obtained by contacting the first raffinate and a polar solvent in a second extraction tower having a column bottom temperature and a top temperature higher than each of the first extraction tower by 10 ° C. or more. A rubber compounding oil obtained by performing a purification treatment including a dewaxing step. Aniline point of 40 to 90 ℃, according to ASTM D3238% C _A of 25 to 45 and% C _N is from 5 to 20, jilsobun is 0.01 mass% or more and a pour point + 30 ℃ or less, the content of the benzo (a) pyrene 1 An extract (A) having a mass ppm or less, a total content of a specific aromatic compound of 10 mass ppm or less, and a kinematic viscosity at 40 ° C of 650 mm 2 / s or more,
Pour point below -10 ℃, aniline point above 70 ℃, the% C _A by ASTM D3238 3 to 20 and% C _N of 15 to 35, jilsobun is 0.01 mass% or less, 90% point 500 ℃ in GC distillation The lube base oil (B) whose flash point is 250 degreeC or more, content of the said benzo (a) pyrene is 1 mass ppm or less, and the total content of the said specific aromatic compound is 10 mass ppm or less.
The manufacturing method of the rubber compounding oil which has a process of mix | blending.

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