JP2013064162A - Lubricant base oil and lubricant composition - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a lubricant base oil having excellent viscosity-temperature characteristics and thermal oxidation stability, compatibly having high viscosity index and low temperature viscosity characteristics at -35°C or lower even when a synthetic oil such as a poly-α-olefin base oil and an ester based base oil and a low viscosity mineral oil are not used and capable of improving MRV viscosity at -40°C and to provide a lubricant composition containing the lubricant base oil.SOLUTION: The lubricant base oil has ≥95 mass% saturated component, and the saturated component has ≤10 mass% cyclic saturated component. The lubricant base oil has a viscosity index of 110 or more, aniline point of 106 or more and 14 to 20% εmethylene occupied in total amount of constituent carbon.

Description

  The present invention relates to a lubricating base oil and a lubricating oil composition.

  Conventionally, in the lubricating oil field, various additives such as highly refined mineral oil and other base oils are blended to improve the characteristics of the lubricating oil such as viscosity-temperature characteristics and thermal / oxidative stability. (For example, refer to Patent Documents 1 to 3).

JP-A-4-36391 Japanese Patent Laid-Open No. 4-68082 Japanese Patent Laid-Open No. 4-120193

  However, recently, the required characteristics of lubricating oils are increasing, and the lubricating base oils described in Patent Documents 1 to 3 are not necessarily sufficient in terms of viscosity-temperature characteristics and thermal / oxidative stability. It can not be said. In particular, in a SAE10 class lubricating base oil and a lubricating oil composition containing this as a main component, a high viscosity index and a low temperature viscosity (CCS viscosity, MRV viscosity, BF viscosity, etc.) at −35 ° C. or lower are used. It is difficult to achieve compatibility at a high level, and it is necessary to use a synthetic base oil such as poly-α-olefin base oil and ester base oil and a lubricating base oil excellent in low temperature viscosity such as a low viscosity mineral oil base oil. is there. However, the above synthetic oils are expensive, and low viscosity mineral base oils generally have a low viscosity index and a high NOACK evaporation amount. When these lubricating base oils are blended, the manufacturing cost of the lubricating oil increases, In addition, it is difficult to achieve a high viscosity index and low evaporation. In addition, when these conventional lubricating base oils are used, there is a limit to the improvement of the above characteristics by the addition of additives.

  The present invention has been made in view of such circumstances, and is excellent in viscosity-temperature characteristics and thermal / oxidative stability, and synthetic oils such as poly-α-olefin base oils and ester base oils, and low viscosity mineral oils. Lubricant base oil that can achieve both high viscosity index and low temperature viscosity characteristics at −35 ° C. or less, and can significantly improve MRV viscosity at −40 ° C. An object is to provide a lubricating oil composition containing an oil base oil.

  In order to solve the above-mentioned problems, the present invention contains 95% by mass or more of the saturated component, the ratio of the cyclic saturated component in the saturated component is 10% by mass or less, the viscosity index is 110 or more, and the aniline point And a ratio of ε-methylene in the total amount of constituent carbon is 14 to 20%, and a lubricating base oil is provided.

  In the lubricating base oil of the present invention, the content of saturated component, the proportion of cyclic saturated component in the saturated component, the viscosity index, the aniline point, and the proportion of ε methylene in the total amount of constituent carbon (hereinafter, depending on circumstances) By simply satisfying the above-mentioned conditions, the “ratio of ε methylene”) can achieve excellent viscosity-temperature characteristics and thermal / oxidative stability. And according to the lubricating base oil of the present invention, it is possible to achieve both a high viscosity index of 130 or more and a low temperature viscosity at −35 ° C. or less, and in particular, the MRV viscosity at −40 ° C. can be remarkably reduced. become. In addition, when an additive is blended in the lubricating base oil, the additive functions at a higher level while the additive is sufficiently stably dissolved and retained in the lubricating base oil. be able to.

  Furthermore, according to the lubricating base oil of the present invention, viscosity resistance and stirring resistance in the practical temperature range can be reduced by the excellent viscosity-temperature characteristics described above, and when a friction modifier or the like is blended. Can maximize its effects. Therefore, the lubricating base oil of the present invention is very useful in that energy loss can be reduced and energy saving can be achieved in a device to which the lubricating base oil is applied.

  According to the present invention, viscosity-temperature characteristics and thermal / oxidation stability are compatible at a high level, and synthetic oils such as poly-α-olefin base oils and ester base oils and low viscosity mineral oil base oils are not used. In both cases, a lubricating base oil and a lubricating oil composition capable of achieving both a high viscosity index and a low temperature viscosity characteristic at −35 ° C. or less, and particularly capable of remarkably improving the MRV viscosity of the lubricating oil at −40 ° C. Provided.

  Hereinafter, preferred embodiments of the present invention will be described in detail.

  The lubricating base oil of the present invention contains 90% by mass or more of the saturated component, the ratio of the cyclic saturated component in the saturated component is 40% by mass or less, the viscosity index is 110 or more, and the aniline point is 106 or more. And the proportion of ε-methylene in the total amount of constituent carbon is 14 to 20%.

  The lubricating base oil of the present invention is not particularly limited as long as the content of the saturated component, the proportion of the cyclic saturated component in the saturated component, the viscosity index, the aniline point, and the proportion of ε methylene satisfy the above conditions. Specifically, a lubricating oil fraction obtained by atmospheric distillation and / or vacuum distillation of crude oil is subjected to solvent removal, solvent extraction, hydrocracking, solvent dewaxing, catalytic dewaxing, hydrorefining, sulfuric acid Among paraffinic mineral oils, or normal paraffinic base oils, isoparaffinic base oils, etc. purified by combining one or more kinds of purification processes such as washing and clay treatment alone or in combination, kinematic viscosity at 100 ° C., Examples include those having a viscosity index and a freezing point that satisfy the above conditions. These lubricating base oils may be used alone or in combination of two or more.

As a preferable example of the lubricating base oil of the present invention, the following base oils (1) to (8) are used as raw materials, and this raw oil and / or a lubricating oil fraction recovered from this raw oil is used in a predetermined manner. The base oil obtained by refine | purifying with a refinement | purification method and collect | recovering lubricating oil fractions can be mentioned.
(1) Distilled oil by atmospheric distillation of paraffinic crude oil and / or mixed base crude oil (2) Distilled oil by vacuum distillation of atmospheric distillation residue of paraffinic crude oil and / or mixed base crude oil ( WVGO)
(3) Wax (such as slack wax) obtained by the lubricant dewaxing process and / or synthetic wax (Fischer-Tropsch wax, GTL wax, etc.) obtained by the gas-liquid (GTL) process, etc.
(4) One or two or more mixed oils selected from base oils (1) to (3) and / or mild hydrocracking treatment oils of the mixed oils (5) selected from base oils (1) to (4) 2 or more kinds of mixed oils (6) Base oil (1), (2), (3), (4) or (5) debris oil (DAO)
(7) Mild hydrocracking treatment oil (MHC) of base oil (6)
(8) Two or more mixed oils selected from base oils (1) to (7).

  The above-mentioned predetermined purification methods include hydrorefining such as hydrocracking and hydrofinishing; solvent refining such as furfural solvent extraction; dewaxing such as solvent dewaxing and catalytic dewaxing; acid clay and activated clay White clay purification; chemical (acid or alkali) cleaning such as sulfuric acid cleaning and caustic soda cleaning is preferable. In the present invention, one of these purification methods may be performed alone, or two or more may be combined. Moreover, when combining 2 or more types of purification methods, the order in particular is not restrict | limited, It can select suitably.

Furthermore, as the lubricating base oil of the present invention, a base oil selected from the above base oils (1) to (8) or a lubricating oil fraction recovered from the base oil is obtained by performing a predetermined treatment. Base oil (9) or (10) is particularly preferred.
(9) The base oil selected from the base oils (1) to (8) or the lubricating oil fraction recovered from the base oil is hydrocracked and recovered from the product or the product by distillation or the like. Hydrocracked mineral oil obtained by performing dewaxing treatment such as solvent dewaxing or catalytic dewaxing on the lubricating oil fraction, or distillation after the dewaxing treatment (10) The above base oils (1) to (8) ) Or a lubricating oil fraction recovered from the base oil is hydroisomerized, and the product or the lubricating oil fraction recovered from the product by distillation or the like is subjected to solvent dewaxing or catalytic dewaxing. Hydroisomerized mineral oil obtained by performing a dewaxing process such as or by distillation after the dewaxing process.

  Moreover, when obtaining the lubricating base oil of (9) or (10) above, a solvent refining treatment and / or a hydrofinishing treatment step may be further provided as necessary at a convenient step.

  The catalyst used for the hydrocracking / hydroisomerization is not particularly limited, but a composite oxide having cracking activity (for example, silica alumina, alumina boria, silica zirconia, etc.) or one of the composite oxides. Hydrogenolysis with a combination of the above combined with a binder and supporting a metal having hydrogenation ability (for example, one or more metals such as Group VIa metal or Group VIII metal in the periodic table) Hydroisomerization catalyst in which a catalyst or a support containing zeolite (for example, ZSM-5, zeolite beta, SAPO-11, etc.) is loaded with a metal having a hydrogenation ability containing at least one of Group VIII metals Are preferably used. The hydrocracking catalyst and the hydroisomerization catalyst may be used in combination by stacking or mixing.

  The reaction conditions in the hydrocracking / hydroisomerization are not particularly limited, but the hydrogen partial pressure is 0.1 to 20 MPa, the average reaction temperature is 150 to 450 ° C., the LHSV is 0.1 to 3.0 hr-1, and the hydrogen / oil ratio. It is preferable to set it as 50-20000 scf / b.

  Preferable examples of the method for producing the lubricating base oil of the present invention include production method A shown below.

That is, the manufacturing method A according to the present invention includes:
NH ₃ to the carrier desorption of the fraction of the NH ₃ is 80% or less at 300 to 800 ° C. relative to the total desorption of NH ₃ in the desorption temperature dependence evaluation, at least one of the periodic table Group VIa metals And a first step of preparing a hydrocracking catalyst on which at least one of the Group VIII metals is supported,
In the presence of a hydrocracking catalyst, a feed oil containing 50% by volume or more of slack wax, hydrogen partial pressure 0.1-14 MPa, average reaction temperature 230-430 ° C., LHSV 0.3-3.0 hr ⁻¹ , hydrogen oil ratio A second step of hydrocracking at 50-14000 scf / b;
A third step of obtaining a lubricating oil fraction by distilling and separating the cracked product oil obtained in the second step;
And a fourth step of dewaxing the lubricating oil fraction obtained in the third step.

  Hereinafter, the production method A will be described in detail.

(Raw oil)
In the production method A, a raw material oil containing 50% by volume or more of slack wax is used. The “raw oil containing 50% by volume or more of slack wax” as used in the present invention is a mixed oil of a raw oil consisting only of slack wax, slack wax and other raw material oil, and 50 volumes of slack wax. % And both raw material oils containing at least% are included.

Slack wax is a wax-containing component by-produced in the solvent dewaxing step when producing a lubricating base oil from a paraffinic lubricating oil fraction. In the present invention, the slack wax is obtained by further deoiling the wax-containing component. Included in wax. The main components of slack wax are n-paraffins and branched paraffins (isoparaffins) with few side chains, and are low in naphthenes and aromatics. The kinematic viscosity of the slack wax used in the preparation of the raw material oil can be appropriately selected according to the kinematic viscosity of the target lubricating base oil, but a low viscosity base oil is produced as the lubricating base oil of the present invention. For this, a relatively low viscosity slack wax having a kinematic viscosity at 100 ° C. of about ² to 25 mm ² / s, preferably about 2.5 to ²⁰ mm ² / s, more preferably about 3 to 15 mm ² / s is desirable. .

  Moreover, although the other property of slack wax is also arbitrary, melting | fusing point becomes like this. Preferably it is 35-80 degreeC, More preferably, it is 45-70 degreeC, More preferably, it is 50-60 degreeC. The oil content of the slack wax is preferably 60% by mass or less, more preferably 50% by mass or less, further preferably 25% by mass or less, particularly preferably 10% by mass or less, and preferably 0.5% by mass. As mentioned above, More preferably, it is 1 mass% or more. The sulfur content of the slack wax is preferably 1% by mass or less, more preferably 0.5% by mass or less, and preferably 0.001% by mass or more.

  Here, the oil content of the fully deoiled slack wax (hereinafter referred to as “slack wax A”) is preferably 0.5 to 10% by mass, more preferably 1 to 8% by mass. The sulfur content of the slack wax A is preferably 0.001 to 0.2% by mass, more preferably 0.01 to 0.15% by mass, and still more preferably 0.05 to 0.12% by mass. On the other hand, the oil content of slack wax (hereinafter referred to as “slack wax B”) that is not deoiled or insufficiently deoiled is preferably 10 to 60% by mass, more preferably 12 to 50% by mass. More preferably, it is 15 to 25% by mass. The sulfur content of the slack wax B is preferably 0.05 to 1% by mass, more preferably 0.1 to 0.5% by mass, and still more preferably 0.15 to 0.25% by mass. The slack waxes A and B may be subjected to a desulfurization treatment depending on the type and characteristics of the hydrocracking / isomerization catalyst, and the sulfur content in that case is preferably 0.01. It is at most mass%, more preferably at most 0.001 mass%.

  The present invention is a highly value-added lubrication having a high viscosity index and excellent low temperature characteristics and thermal / oxidative stability even when slack wax having a relatively high oil content and sulfur content, and relatively poor and inexpensive is used as a raw material. It is very useful in that an oil base oil can be obtained.

  When the raw material oil is a mixed oil of slack wax and other raw material oil, the other raw material oil is not particularly limited as long as the ratio of slack wax to the total amount of the mixed oil is 50% by volume or more. A heavy oil-distilled distillate and / or a mixed oil of vacuum-distilled distillate is preferably used.

  Further, when the raw material oil is a mixed oil of slack wax and another raw material oil, the ratio of slack wax in the mixed oil is more preferably 70% by volume or more from the viewpoint of producing a base oil having a high viscosity index. 75% by volume or more is even more preferable. When the ratio is less than 50% by volume, the oil base such as aromatics and naphthenes in the obtained lubricating base oil tends to increase and the viscosity index of the lubricating base oil tends to decrease.

  On the other hand, the heavy atmospheric distillation distillate and / or vacuum distillation distillate of crude oil used in combination with slack wax has a distillation temperature of 300 to 570 ° C. in order to keep the viscosity index of the lubricating base oil produced high. A fraction having a distillate component of 60% by volume or more in the range is preferable.

(Hydrocracking catalyst)
In the manufacturing method A, the carrier desorption of the fraction of the NH ₃ is 80% or less at 300 to 800 ° C. relative to the total desorption of NH ₃ in the NH ₃ desorption temperature dependence evaluation, periodic table Group VIa A hydrocracking catalyst in which at least one of the metals and at least one of the Group VIII metals is supported is used.

Here, “NH ₃ desorption temperature dependency evaluation” refers to literature (Sawa M., Niwa M., Murakami Y., Zeolites 1990, 10, 532, Karge HG, Dondur V., J. Phys. Chem., 1990, 94, 765, etc.) and is performed as follows. First, the catalyst carrier is pretreated at a temperature of 400 ° C. or higher for 30 minutes or more under a nitrogen stream to remove adsorbed molecules, and then adsorbs NH ₃ at 100 ° C. until saturation. Then, the catalyst support to 100 to 800 ° C. 10 ° C. / min was heated by the following heating rate desorbed NH _3, to monitor the NH ₃ separated at every predetermined temperature by desorption. Then, the fraction of the NH ₃ desorption amount at 300 ° C. to 800 ° C. with respect to the total NH ₃ desorption amount (desorption amount at 100 to 800 ° C.) is obtained.

The catalyst carrier used in the production method A are those desorption of the fraction of NH ₃ at 300 to 800 ° C. relative to the total desorption of NH ₃ in the NH ₃ desorption temperature dependence evaluation of the following 80% , Preferably 70% or less, more preferably 60% or less. By constituting a hydrocracking catalyst using such a carrier, the acid properties that govern the cracking activity are sufficiently suppressed, so that the high molecular weight n-paraffin derived from slack wax or the like in the raw oil by hydrocracking. The production of isoparaffin by decomposition isomerization can be performed efficiently and reliably, and excessive decomposition of the produced isoparaffin compound can be sufficiently suppressed. As a result, a sufficient amount of molecules having a moderately branched chemical structure and a high viscosity index can be provided in an appropriate molecular weight range.

  As such a support, a binary oxide which is amorphous and has an acid property is preferable. For example, it is exemplified in the literature ("Metal oxide and its catalytic action", Tetsuro Shimizu, Kodansha, 1978). And binary oxides.

Among them, an amorphous composite oxide which is an acid composed of two kinds of oxides of elements selected from Al, B, Ba, Bi, Cd, Ga, La, Mg, Si, Ti, W, Y, Zn and Zr. It is preferable to contain a property binary oxide. By adjusting the ratio of each oxide of these acid property binary oxides, a support having an acid property suitable for this purpose can be obtained in the NH ₃ adsorption / desorption evaluation. In addition, the acid property binary oxide constituting the carrier may be one of the above or a mixture of two or more. Further, the carrier may be composed of the above-mentioned acid property binary oxide, or may be a carrier obtained by binding the acid property binary oxide with a binder.

  Further, the carrier is amorphous silica / alumina, amorphous silica / zirconia, amorphous silica / magnesia, amorphous silica / titania, amorphous silica / boria, amorphous alumina / zirconia, amorphous alumina / magnesia, amorphous At least one selected from alumina / titania, amorphous alumina / boria, amorphous zirconia / magnesia, amorphous zirconia / titania, amorphous zirconia / boria, amorphous magnesia / titania, amorphous magnesia / boria and amorphous titania / boria It is preferable to contain two kinds of acid nature binary oxides. The acidic binary oxide constituting the carrier may be one of the above or a mixture of two or more. Further, the carrier may be composed of the above-mentioned acid property binary oxide, or may be a carrier obtained by binding the acid property binary oxide with a binder. The binder is not particularly limited as long as it is generally used for catalyst preparation, but is preferably selected from silica, alumina, magnesia, titania, zirconia, clay, or a mixture thereof.

  In the production method A described above, the carrier is composed of at least one of group VIa metals (molybdenum, chromium, tungsten, etc.) of the periodic table and group VIII metal (nickel, cobalt, palladium, platinum, etc.). At least one of them is supported to form a hydrocracking catalyst. These metals are responsible for hydrogenation ability, terminate the reaction in which the paraffinic compound is decomposed or branched by the acidic carrier, and play an important role in producing isoparaffin having an appropriate molecular weight and branched structure.

  As the amount of metal supported in the hydrocracking catalyst, the supported amount of Group VIa metal is 5 to 30% by mass per one type of metal, and the supported amount of Group VIII metal is 0.2 to 10% by mass per one type of metal. % Is preferred.

  Further, in the hydrocracking catalyst used in the production method A, molybdenum is contained in the range of 5 to 30% by mass as one or more metals of the Group VIa metal, and one or more of the Group VIII metals is contained. More preferably, the metal contains nickel in the range of 0.2 to 10% by mass.

  The hydrocracking catalyst composed of the above support and one or more metals of Group VIa metal and one or more metals of Group VIII metal is preferably used for hydrocracking in a sulfurized state. The sulfurization treatment can be performed by a known method.

(Hydrolysis process)
In the production method A, a raw material oil containing 50% by volume or more of slack wax in the presence of the hydrocracking catalyst has a hydrogen partial pressure of 0.1 to 14 MPa, preferably 1 to 14 MPa, more preferably 2 to 2. 7 MPa; average reaction temperature of 230 to 430 ° C., preferably 330 to 400 ° C., more preferably 350 to 390 ° C .; LHSV of 0.3 to 3.0 hr ⁻¹ , preferably 0.5 to 2.0 hr ⁻¹ ; Hydrogenolysis is performed at a hydrogen oil ratio of 50 to 14,000 scf / b, preferably 100 to 5000 scf / b.

  In such a hydrocracking process, isomerization to isoparaffin progresses in the process of cracking n-paraffin derived from slack wax in the raw material oil, thereby producing an isoparaffin component having a low pour point and a high viscosity index. At the same time, it breaks down aromatic compounds, which are inhibitors of high viscosity index contained in the feedstock, into monocyclic aromatic compounds, naphthene compounds and paraffin compounds, and inhibits high viscosity index. The polycyclic naphthene compound as a factor can be decomposed into a monocyclic naphthene compound or a paraffin compound. From the viewpoint of increasing the viscosity index, it is preferable that the raw material oil contains fewer compounds having a high boiling point and a low viscosity index.

Further, the decomposition rate for evaluating the progress of the reaction is expressed by the following formula:
(Decomposition rate (volume%)) = 100− (ratio of the fraction having a boiling point of 360 ° C. or more in the product (volume%))
In this way, the decomposition rate is preferably 3 to 90% by volume. When the decomposition rate is less than 3% by volume, isoparaffins are generated by decomposition and isomerization of high-molecular-weight n-paraffins having a high pour point contained in the feedstock, and hydrocracking of aromatics and polycyclic naphthenes with poor viscosity index. When the decomposition rate exceeds 90% by volume, the yield of the lubricating oil fraction decreases, which is not preferable.

(Distillation separation process)
Next, the lubricating oil fraction is distilled and separated from the cracked product oil obtained by the hydrocracking step. At this time, a fuel oil fraction may be obtained as a light component.

  The fuel oil fraction is a fraction obtained as a result of sufficient desulfurization and denitrogenation, and sufficient aromatic hydrogenation. Among these, the naphtha fraction has a high isoparaffin content, the kerosene fraction has a high smoke point, and the light oil fraction has a high cetane number.

  On the other hand, when hydrocracking in the lubricating oil fraction is insufficient, a part of it may be subjected to the hydrocracking process again. Further, in order to obtain a lubricating oil fraction having a desired kinematic viscosity, the lubricating oil fraction may be further distilled under reduced pressure. This vacuum distillation separation may be performed after the dewaxing treatment described below.

  In the evaporative separation step, a lubricant base oil called 70 Pale, SAE10, or SAE20 can be suitably obtained by distilling the cracked product oil obtained in the hydrocracking step under reduced pressure.

  A system that uses slack wax with lower viscosity as the feedstock is suitable for producing a large amount of 70 Pale and 10 SAE fractions, and a system that uses slack wax with a high viscosity within the above range as feedstock produces a lot of SAE20. Suitable for doing. However, even if a high-viscosity slack wax is used, conditions for generating a considerable amount of 70 Pale and SAE 10 can be selected depending on the progress of the decomposition reaction.

(Dewaxing process)
In the above-described distillation separation step, the lubricating oil fraction fractionated from the cracked product oil has a high pour point, and is dewaxed to obtain a lubricating base oil having a desired freezing point. The dewaxing treatment can be performed by a usual method such as a solvent dewaxing method or a contact dewaxing method. Among these, the solvent dewaxing method generally uses a mixed solvent of MEK and toluene, but may use a solvent such as benzene, acetone, MIBK or the like. In order to improve the low temperature viscosity characteristics of the dewaxed oil of the obtained SAE 10 class fraction, the solvent / oil ratio is preferably 1 to 6 times, and the filtration temperature is −25 ° C. or lower. It is preferably −26 to −45 ° C., more preferably −27 to −40 ° C., and particularly preferably −28 to −35 ° C. The wax removed here can be used again as a slack wax in the hydrocracking step.

  In the said manufacturing method, you may add a solvent refinement | purification process and / or a hydrorefining process to a dewaxing process. These additional treatments are performed in order to improve the ultraviolet stability and oxidation stability of the lubricating base oil, and can be carried out by a method used in a normal lubricating oil refining process.

  In the solvent purification, furfural, phenol, N-methylpyrrolidone or the like is generally used as a solvent, and a small amount of aromatic compounds, particularly polycyclic aromatic compounds remaining in the lubricating oil fraction are removed.

In addition, hydrorefining is performed to hydrogenate olefin compounds and aromatic compounds, and the catalyst is not particularly limited. However, at least one of Group VIa metals such as molybdenum, cobalt, nickel, etc. Using an alumina catalyst supporting at least one of the Group VIII metals, the reaction pressure (hydrogen partial pressure) is 7 to 16 MPa, the average reaction temperature is 300 to 390 ° C., and the LHSV is 0.5 to 4.0 hr ⁻¹ . Can be done below.

  Moreover, as a preferable example of the method for producing the lubricating base oil of the present invention, the following production method B can be mentioned.

That is, the production method B according to the present invention is:
A fifth step of hydrocracking and / or hydroisomerizing a feedstock containing paraffinic hydrocarbons in the presence of a catalyst;
A sixth step of dewaxing the product obtained in the fifth step or the lubricating oil fraction recovered from the product by distillation or the like;
Is provided.

  Hereinafter, the production method B will be described in detail.

(Raw oil)
In the production method B, a raw material oil containing paraffinic hydrocarbon is used. The “paraffinic hydrocarbon” referred to in the present invention means a hydrocarbon having a paraffin molecule content of 70% by mass or more. The carbon number of the paraffinic hydrocarbon is not particularly limited, but usually about 10 to 100 is used. The paraffinic hydrocarbon production method is not particularly limited, and various paraffinic hydrocarbons such as petroleum and synthetic can be used. Particularly preferable paraffinic hydrocarbons include a gas-liquid (GTL) process and the like. Synthetic waxes obtained (Fischer-Tropsch wax (FT wax), GTL wax, etc.) can be mentioned, among which FT wax is preferred. The synthetic wax is preferably a wax containing, as a main component, a normal paraffin having 15 to 80 carbon atoms, more preferably 20 to 50 carbon atoms.

The kinematic viscosity of the paraffinic hydrocarbon used in the preparation of the raw material oil can be appropriately selected according to the kinematic viscosity of the target lubricating base oil, but a low viscosity base oil is used as the lubricating base oil of the present invention. For production, a relatively low-viscosity paraffinic system having a kinematic viscosity at 100 ° C. of about ² to 25 mm ² / s, preferably about 2.5 to ²⁰ mm ² / s, more preferably about 3 to 15 mm ² / s. Hydrocarbons are desirable. In addition, other properties of the paraffinic hydrocarbon are optional, but when the paraffinic hydrocarbon is a synthetic wax such as FT wax, the melting point is preferably 35 to 80 ° C, more preferably 50 to 80 ° C, More preferably, it is 60-80 degreeC. The oil content of the synthetic wax is preferably 10% by mass or less, more preferably 5% by mass or less, and further preferably 2% by mass or less. Further, the sulfur content of the synthetic wax is preferably 0.01% by mass or less, more preferably 0.001% by mass or less, and further preferably 0.0001% by mass or less.

  When the raw material oil is a mixed oil of the above synthetic wax and another raw material oil, the other raw material oil is not particularly limited as long as the ratio of the synthetic wax to the total amount of the mixed oil is 50% by volume or more. A heavy atmospheric distillation oil and / or a mixed oil of reduced pressure distillation oil is preferably used.

  Further, when the raw material oil is a mixed oil of the above synthetic wax and other raw material oils, the proportion of the synthetic wax in the mixed oil is more than 70% by volume from the viewpoint of producing a base oil having a high viscosity index. Preferably, 75% by volume or more is even more preferable. If the ratio is less than 70% by volume, the lubricating base oil to be obtained tends to increase the oil content such as aromatics and naphthenes and decrease the viscosity index of the lubricating base oil.

  On the other hand, heavy crude pressure distillation distillate and / or vacuum distillation distillate of crude oil used in combination with synthetic wax is used at a distillation temperature of 300 to 570 ° C. in order to keep the viscosity index of the lubricating base oil to be produced high. A fraction having a distillate component of 60% by volume or more in the range is preferable.

(catalyst)
The catalyst used in production method B is not particularly limited, but a catalyst in which at least one selected from Group VI metal and Group VIII metal of the periodic table as an active metal component is supported on a support containing aluminosilicate. Preferably used.

  Aluminosilicate refers to a metal oxide composed of three elements of aluminum, silicon, and oxygen. Further, other metal elements can be allowed to coexist within a range that does not hinder the effects of the present invention. In this case, the amount of the other metal element is preferably 5% by mass or less, and more preferably 3% by mass or less of the total amount of alumina and silica as the oxide. Examples of metal elements that can coexist include titanium, lanthanum, manganese, and the like.

The crystallinity of aluminosilicate can be estimated by the proportion of tetracoordinate aluminum atoms in all aluminum atoms, and this proportion can be measured by ²⁷ Al solid state NMR. As the aluminosilicate used in the present invention, the ratio of tetracoordinated aluminum to the total amount of aluminum is preferably 50% by mass or more, more preferably 70% by mass or more, and further preferably 80% by mass or more. Hereinafter, an aluminosilicate having a ratio of tetracoordinated aluminum to the total amount of aluminum of 50% by mass or more is referred to as “crystalline aluminosilicate”.

  As the crystalline aluminosilicate, so-called zeolite can be used. Preferable examples include Y-type zeolite, ultrastable Y-type zeolite (USY-type zeolite), β-type zeolite, mordenite, ZSM-5, etc. Among them, USY zeolite is particularly preferable. In the present invention, one type of crystalline aluminosilicate may be used alone, or two or more types may be used in combination.

  Examples of a method for preparing a carrier containing crystalline aluminosilicate include a method of molding a mixture of crystalline aluminosilicate and a binder and firing the molded body. The binder to be used is not particularly limited, but alumina, silica, silica alumina, titania and magnesia are preferable, and alumina is particularly preferable. The use ratio of the binder is not particularly limited, but is usually preferably 5 to 99% by mass and more preferably 20 to 99% by mass based on the total amount of the molded body. 430-470 degreeC is preferable, as for the baking temperature of the molded object containing a crystalline aluminosilicate and a binder, 440-460 degreeC is more preferable, and 445-455 degreeC is more preferable. The firing time is not particularly limited, but is usually 1 minute to 24 hours, preferably 10 minutes to 20 hours, more preferably 30 minutes to 10 hours. Firing may be performed in an air atmosphere, but is preferably performed in an oxygen-free atmosphere such as a nitrogen atmosphere.

  Examples of the Group VI b metal supported on the carrier include chromium, molybdenum, tungsten, and the like. Specific examples of the Group VIII metal include cobalt, nickel, rhodium, palladium, iridium, platinum, and the like. It is done. These metals may be used individually by 1 type, or may be used in combination of 2 or more types. When two or more kinds of metals are combined, noble metals such as platinum and palladium may be combined, base metals such as nickel, cobalt, tungsten and molybdenum may be combined, or a noble metal and a base metal may be combined.

  Further, the loading of the metal on the carrier can be performed by information such as impregnation of the carrier into a solution containing the metal, ion exchange, and the like. The amount of the metal supported can be appropriately selected, but is usually 0.05 to 2% by mass, preferably 0.1 to 1% by mass based on the total amount of the catalyst.

(Hydrolysis / Hydroisomerization process)
In the production method B, the feedstock oil containing paraffinic hydrocarbon is hydrocracked / hydroisomerized in the presence of the catalyst. Such hydrocracking / hydroisomerization step can be performed using a fixed bed reactor. As conditions for hydrocracking / hydroisomerization, for example, the temperature is preferably 250 to 400 ° C., the hydrogen pressure is preferably 0.5 to 10 MPa, and the liquid space velocity (LHSV) of the feedstock is preferably 0.5 to 10 h ^−1. .

(Distillation separation process)
Next, the lubricating oil fraction is distilled and separated from the cracked product oil obtained by the hydrocracking / hydroisomerization step. In addition, since the distillation separation process in the manufacturing method B is the same as the distillation separation process in the manufacturing method A, the overlapping description is abbreviate | omitted here.

(Dewaxing process)
Subsequently, the lubricating oil fraction fractionated from the cracked product oil in the distillation separation step is dewaxed. Such a dewaxing step can be performed using a conventionally known dewaxing process such as solvent dewaxing or catalytic dewaxing. Here, if the substance having a boiling point of 370 ° C. or less present in the cracked / isomerized product oil is not separated from the high boiling point substance prior to dewaxing, depending on the use of the cracked / isomerized product oil, The compound may be dewaxed or a fraction having a boiling point of 370 ° C. or higher may be dewaxed.

  In solvent dewaxing, the hydroisomerized product is contacted with chilled ketone and acetone, and other solvents such as MEK, MIBK, and further cooled to precipitate the high pour point material as a waxy solid, which is precipitated with raffinate. Separate from a solvent-containing lubricating oil fraction. Further, the raffinate can be cooled with a scraped surface chiller to remove wax solids. Low molecular weight hydrocarbons such as propane can also be used for dewaxing. In this case, the cracked / isomerized product oil and the low molecular weight hydrocarbon are mixed and at least a part thereof is vaporized to decompose / isomerize. The product oil is further cooled to precipitate the wax. The wax is separated from the raffinate by filtration, membrane or centrifugation. Thereafter, the solvent is removed from the raffinate, and the raffinate is fractionally distilled to obtain the target lubricating base oil.

  In the case of catalytic dewaxing (catalyst dewaxing), the cracked / isomerized product oil is reacted with hydrogen in the presence of a suitable dewaxing catalyst under conditions effective to lower the pour point. In catalytic dewaxing, some of the high-boiling substances in the cracking / isomerization product are converted to low-boiling substances, the low-boiling substances are separated from the heavier base oil fraction, and the base oil fraction is fractionated. Two or more kinds of lubricating base oils are obtained. The low-boiling substances can be separated before obtaining the target lubricating base oil or during fractional distillation.

  The dewaxing catalyst is not particularly limited as long as the freezing point of the obtained SAE10 class fraction dewaxing oil can be set to -25 ° C. or lower. What can obtain lube base oil is preferable. As such a dewaxing catalyst, a shape selective molecular sieve (molecular sieve) is preferable. Specifically, ferrierite, mordenite, ZSM-5, ZSM-11, ZSM-23, ZSM-35, ZSM-22 ( And theta aluminophosphates (SAPO) and the like. These molecular sieves are preferably used in combination with a catalytic metal component, and more preferably in combination with a noble metal. A preferable combination includes, for example, a composite of platinum and H-mordenite.

The dewaxing conditions are not particularly limited, but the temperature is preferably 200 to 500 ° C., and the hydrogen pressure is preferably 10 to 200 bar (1 MPa to 20 MPa). In the case of a flow-through reactor, the H ₂ treatment rate is preferably 0.1 to 10 kg / l / hr, and the LHSV is preferably 0.1 to 10 ^{−1 and} more preferably 0.2 to 2.0 h ^−1. . Dewaxing refers to a substance having an initial boiling point of 350 to 400 ° C., usually 40% by mass or less, preferably 30% by mass or less, contained in the cracked / isomerized product oil, having a boiling point lower than the initial boiling point. It is preferable to carry out the conversion to a substance having the same.

  As mentioned above, although the manufacturing method A and the manufacturing method B which are the preferable manufacturing methods of the lubricating base oil of this invention were demonstrated, the manufacturing method of the lubricating base oil of this invention is not limited to these. For example, in the above production method A, synthetic waxes such as FT wax and GTL wax may be used instead of slack wax. In the production method B, a raw material oil containing slack wax (preferably slack wax A, B) may be used. Furthermore, in each of the production methods A and B, slack wax (preferably slack wax A and B) and synthetic wax (preferably FT wax and GTL wax) may be used in combination.

  In addition, when the raw material oil used when producing the lubricating base oil of the present invention is a mixed oil of the above slack wax and / or synthetic wax and a raw material oil other than these waxes, slack wax and The content of the synthetic wax is preferably 50% by mass or more based on the total amount of the raw material oil.

  The raw material oil for producing the lubricating base oil of the present invention is a raw material oil containing slack wax and / or synthetic wax, and the oil content is preferably 60% by mass or less, more preferably 50% by mass. In the following, it is more preferable that the raw material oil is 25% by mass or less.

  Hereinafter, the lubricating base oil of the present invention will be further described in detail.

  The content of the saturated component in the lubricating base oil of the present invention is 90% by mass or more, preferably 95% by mass or more, more preferably 97% by mass or more, as described above, based on the total amount of the lubricating base oil. Preferably it is 98 mass% or more. The proportion of the cyclic saturated component in the saturated component is 40% by mass or less as described above, preferably 30% by mass or less, more preferably 25% by mass or less, still more preferably 20% by mass or less, and still more preferably. It is 10 mass% or less, Most preferably, it is 5 mass% or less. When the content of the saturated component and the ratio of the cyclic saturated component in the saturated component satisfy the above-mentioned conditions, and the ratio of the viscosity index, the aniline point, and ε-methylene respectively satisfy the specific conditions, the viscosity-temperature characteristics and heat / Oxidation stability can be achieved and high viscosity index and excellent at −35 ° C. or lower without using synthetic oil such as poly-α-olefin base oil and ester base oil and low viscosity mineral oil base oil It becomes possible to achieve both low temperature viscosity characteristics. In addition, when an additive is blended in the lubricating base oil, the additive functions at a higher level while the additive is sufficiently stably dissolved and retained in the lubricating base oil. be able to. Furthermore, when the content of the saturated component and the ratio of the cyclic saturated component in the saturated component satisfy the above conditions, the friction characteristics of the lubricating base oil itself can be improved, and as a result, the friction reducing effect is improved. As a result, energy saving can be improved.

  When the content of the saturated component is less than 90% by mass, the heat / oxidation stability, the viscosity-temperature characteristic, and the friction characteristic are insufficient. Moreover, when the ratio of the cyclic | annular saturated part to a saturated part exceeds 40 mass%, when an additive is mix | blended with lubricating base oil, the effect | action of the said additive will fall.

  In the lubricating base oil of the present invention, the fact that the cyclic saturated component in the saturated component is 40% by mass or less is equivalent to the non-cyclic saturated component in the saturated component being 60% by mass or more. Here, the non-cyclic saturated component includes both a linear paraffin component and a branched paraffin component. The ratio of each paraffin component in the lubricating base oil of the present invention is not particularly limited, but the ratio of the branched paraffin component is preferably 54 to 99.9% by mass, more preferably 80 to 90%, based on the total amount of the lubricating base oil. 99.5 mass%, More preferably, it is 95-99 mass%, Most preferably, it is 97-99 mass%. When the proportion of the branched paraffin in the lubricating base oil satisfies the above conditions, the thermal / oxidative stability and viscosity-temperature characteristics can be further improved, and an additive is added to the lubricating base oil. In this case, the function of the additive can be expressed at a higher level while the additive is sufficiently and stably dissolved and held.

  Further, in the lubricating base oil of the present invention, the content of monocyclic saturated component and saturated component of two or more rings in the saturated component is not particularly limited as long as the total is 40% by mass or less, The proportion of the saturated portion occupied by two or more rings is preferably 20% by mass or less, more preferably 15% by mass or less, and still more preferably 11% by mass or less. Further, the ratio of the saturated component of two or more rings in the saturated component is preferably 0.5% by mass or more, more preferably 0.8% by mass or more, and further preferably 1% by mass or more. preferable. Further, the percentage of saturated one ring in the saturated content may be 0% by mass, preferably 0.1% by mass or more, and preferably 20% by mass or less, more preferably 10% by mass or less. More preferably, it is 5% by mass or less, particularly preferably 3% by mass or less.

In the lubricating base oil of the present invention, the ratio (M _A / M _B ) between the mass (M _A ) of the monocyclic saturated component contained in the cyclic saturated component and the mass (M _B ) of the saturated component of two or more rings. Is preferably 20 or less, more preferably 3 or less, still more preferably 2 or less, still more preferably 1 or less, and particularly preferably 0.5 or less. _Further, M A / _{M B} may be zero, it is preferably at least 0.01, more preferably 0.05 or more. By the above condition is satisfied M A _/ M _B, the viscosity - a temperature characteristic and heat and oxidation stability can be further compatible at a high level.

  In addition, content of the saturated part said by this invention means the value (unit: mass%) measured based on ASTM D 2007-93.

  Further, the ratios of the cyclic saturated component, the single ring saturated component, the two or more saturated components and the non-cyclic saturated component in the saturated component as used in the present invention are naphthenic components measured in accordance with ASTM D 2786-91, respectively. (Measuring target: 1-ring to 6-ring naphthene, unit: mass%) and alkane content (unit: mass%).

In addition, the linear paraffin content in the lubricating base oil referred to in the present invention is the gas chromatographic analysis of the saturated content separated and separated by the method described in ASTM D 2007-93 under the following conditions. The value obtained by converting the measured value when the linear paraffin content in the saturated content is identified and quantified based on the total amount of the lubricating base oil is meant. In the identification and quantification, a mixed sample of straight-chain paraffin having 5 to 50 carbon atoms is used as a standard sample, and the straight-chain paraffin content in the saturated portion is the total peak area value of the chromatogram (in the diluent). It is determined as the ratio of the sum of peak area values corresponding to each linear paraffin to (excluding the peak area value derived from).
(Gas chromatography conditions)
Column: non-polar liquid phase column (length 25 mm, inner diameter 0.3 mmφ, liquid phase film thickness 0.1 μm)
Temperature rising condition: 50 ° C. to 400 ° C. (temperature rising rate: 10 ° C./min)
Carrier gas: helium (linear velocity: 40 cm / min)
Split ratio: 90/1
Sample injection amount: 0.5 μL (injection amount of sample diluted 20 times with carbon disulfide)

  The ratio of branched paraffin in the lubricating base oil is the difference between the non-cyclic saturated content in the saturated content and the linear paraffin content in the saturated content, converted based on the total amount of the lubricating base oil. Means the value.

  It should be noted that a similar method for obtaining the result for the number can be used in the separation method of the saturated component or the composition analysis of the cyclic saturated component and the non-cyclic saturated component. For example, in addition to the above, a method described in ASTM D 2425-93, a method described in ASTM D 2549-91, a method using high performance liquid chromatography (HPLC), a method obtained by improving these methods, and the like can be given.

  In addition, the aromatic content in the lubricating base oil of the present invention is such that the content of the saturated content, the ratio of the cyclic saturated content in the saturated content, the viscosity index, the aniline point, and the ratio of ε-methylene satisfy the above conditions. If it is a thing, it will not restrict | limit in particular, Preferably it is 5 mass% or less on the basis of the lubricant base oil whole quantity, More preferably, it is 4 mass% or less, More preferably, it is 3 mass% or less, Preferably it is 0.1 It is at least 0.5% by mass, more preferably at least 0.5% by mass, even more preferably at least 1% by mass, particularly preferably at least 1.5% by mass. If the aromatic content exceeds the above upper limit, the viscosity-temperature characteristics, thermal / oxidative stability, friction characteristics, volatilization prevention characteristics and low-temperature viscosity characteristics tend to decrease. When an additive is blended with the additive, the effectiveness of the additive tends to decrease. Further, the lubricating base oil of the present invention may not contain an aromatic component, but the solubility of the additive can be further improved by setting the aromatic content to be equal to or higher than the above lower limit value. it can.

  In addition, content of aromatic content as used in the field of this invention means the value measured based on ASTM D 2007-93. In general, the aromatic component includes alkylbenzene, alkylnaphthalene, anthracene, phenanthrene and alkylated products thereof, as well as compounds in which four or more benzene rings are condensed, pyridines, quinolines, phenols and naphthols. Aromatic compounds having atoms are included.

  Further, as described above, the viscosity index of the lubricating base oil of the present invention is 110 or more, preferably 120 or more, more preferably 130 or more, still more preferably 135 or more, and particularly preferably 138 or more. When the viscosity index is less than 110, the viscosity-temperature characteristic becomes insufficient, and further, the heat / oxidation stability and further the volatilization prevention property are lowered. In addition, the viscosity index as used in the field of this invention means the viscosity index measured based on JISK2283-1993.

  The aniline point (AP (° C.)) of the lubricating base oil of the present invention is 106 ° C. or higher as described above, preferably 110 ° C. or higher, more preferably 115 ° C. or higher, and still more preferably 118 ° C. or higher. . If the aniline point is less than the above lower limit, the viscosity-temperature characteristics and thermal / oxidative stability, as well as volatilization prevention and low-temperature viscosity characteristics are reduced, and when an additive is added to the lubricating base oil. The effectiveness of the additive is reduced. In addition, the aniline point as used in the field of this invention means the aniline point measured based on JISK2256-1985.

  Further, the proportion of ε-methylene in the total amount of constituent carbon of the lubricating base oil of the present invention is 14 to 20% as described above, preferably 14.5 to 19%, more preferably 15 to 18%, particularly Preferably it is 15 to 17%. If the ε-methylene ratio is less than 14%, the viscosity-temperature characteristics and thermal / oxidative stability will decrease, and if it exceeds 20%, the low-temperature viscosity characteristics tend to decrease, and if it exceeds 25%, it will deteriorate significantly. To do. On the other hand, as another aspect of the present invention, when the ratio of ε methylene exceeds 20% and is 25% or less, preferably 20.5 to 24%, the viscosity index is 140 or more and 160 or less, preferably 142 to 150. It is also possible to obtain a lubricating base oil having sufficient low-temperature viscosity characteristics and thermal / oxidative stability. Such a lubricating base oil can have a CCS viscosity at −35 ° C. of less than 3000 mPa · s, preferably 2200 to 2900 mPa · s, more preferably 2300 to 2800 mPa · s. The lubricating oil composition using oil may have an MRV viscosity at −40 ° C. of 60000 mPa · s or less, preferably 40000 mPa · s or less.

The ratio of ε-methylene in the total amount of constituent carbon of the lubricating base oil of the present invention is the ratio of the total integrated intensity attributed to the CH ₂ main chain to the total integrated intensity of all carbon, as measured by ¹³ C-NMR. However, other methods may be used as long as an equivalent result is obtained. In the present invention, at the time of ¹³ C-NMR measurement, 0.5 g of a sample diluted with 3 g of deuterated chloroform was used as a sample, the measurement temperature was room temperature, and the resonance frequency was 100 MHz. Moreover, the measuring method used the coupling method with a gate.

By the above analysis method,
(A) Sum of integral intensities with chemical shifts of about 10-50 ppm (sum of integral intensities due to all constituent carbons), and (b) Sum of integral intensities with chemical shifts of 29.7-30.0 ppm (causes ε methylene) Total integrated intensity)
Are measured, and the ratio (%) of (b) when (a) is taken as 100% is calculated. The ratio of (b) shows the ratio of ε methylene to the total amount of constituent carbon of the lubricating base oil.

The ratio of ε-methylene is 4 carbon atoms (α carbon, β carbon, γ carbon, δ) from the molecular and branched ends on the main chain having a specific chemical shift (α, β, γ, δ) in NMR. The ratio of carbon atoms derived from carbon atoms on the main chain excluding (carbon) and having a certain chemical shift (ε) is shown. When the molecular weight (or average molecular weight) of the lubricating base oil is about the same, a large proportion of ε methylene corresponds to a long chain length of CH ₂ chains with few branches or no branches on the main chain. In addition, a small proportion of ε-methylene corresponds to a short CH ₂ chain length with many branches or no branches on the main chain.

Further, the proportion of tertiary carbon in the total amount of constituent carbon of the lubricating base oil of the present invention is not particularly limited, but is preferably 1 to 15%, more preferably 5 to 12%, and further preferably 6 to 10%.
%. By setting the proportion of tertiary carbon within the above range, a lubricating base oil having excellent viscosity temperature characteristics and thermal / oxidation stability can be obtained. In the present invention, when the proportion of tertiary carbon in the total amount of constituent carbon of the lubricating base oil is 5 to 8%, preferably 6 to 7%, the viscosity index is higher, and CCS at -35 ° C. Lower viscosity, smaller NOACK evaporation,
When the proportion of the tertiary carbon is 8 to 10%, preferably 9 to 10%, M at −40 ° C.
A lubricating oil composition having a lower RV viscosity and an excellent acid value increase inhibiting effect in the presence of NOx can be obtained. Here, the proportion of tertiary carbon means the proportion of carbon atoms attributed to> CH- in the total amount of constituent carbon, that is, the proportion of carbon atoms attributed to branching or naphthene.

The ratio of tertiary carbon means the ratio of the total integrated intensity due to tertiary carbon to the total integrated intensity of all carbons measured by ¹³ C-NMR as described above, but an equivalent result was obtained. Other methods may be used as long as possible.

By the above analysis method,
(A) total of chemical intensities of about 10-50 ppm chemical shift (sum of integrated intensities due to all constituent carbons), and (c) chemical shifts of 27.9-28.1 ppm, 28.4-28.6 ppm, 32 6.3 to 33.2 ppm, 34.4 to 34.6 ppm, 37.4 to 37.6 ppm, 38.8 to 39.1 ppm, 40.4 to 40.6 ppm of total integrated intensity (methyl group, ethyl group and Other integrated strengths due to tertiary carbon and naphthene tertiary carbon combined with other branching machines)
Are measured, and the ratio (%) of (c) where (a) is 100% is calculated. The ratio of (c) indicates the ratio of tertiary carbon to the total amount of constituent carbon of the lubricating base oil.

Further, the proportion of carbon derived from the terminal methyl group (—CH ₃ ) in the total amount of constituent carbon of the lubricating base oil of the present invention is not particularly limited, but is preferably 10 to 20%, more preferably 12 to 18 %, More preferably 14 to 16%. By setting the proportion of carbon attributed to the terminal methyl group within the above range, a lubricating base oil having excellent viscosity-temperature characteristics and thermal / oxidation stability can be obtained.

In addition, the ratio of the carbon resulting from the terminal methyl group means the ratio of the total integrated intensity attributed to the carbon attributed to the terminal methyl group to the total integrated intensity of all the carbons measured by ¹³ C-NMR. However, other methods may be used as long as equivalent results can be obtained.

By the above analysis method,
(A) the total integrated intensity of chemical shifts of about 10-50 ppm (total integrated intensity due to all constituent carbons), and (d) chemical shifts of 10.7-11.6 ppm, 13.8-14.7 ppm, 19 .2～20.1Ppm, the sum of integrated intensity of 22.5～22.8Ppm (terminal ethyl groups (total integrated intensity attributed to the carbon atoms resulting from -CH ₃₎₎
Are measured, and the ratio (%) of (d) when (a) is taken as 100% is calculated. The proportion of (d) indicates the proportion of carbon atoms attributed to terminal methyl groups with respect to the total amount of constituent carbon of the lubricating base oil.

  The other physical properties and composition of the lubricating base oil of the present invention are not particularly limited as long as the content of the saturated component, the proportion of the cyclic saturated component in the saturated component, the viscosity index, the aniline point, and the proportion of ε-methylene satisfy the above conditions. However, regarding the carbon number distribution of the lubricating base oil of the present invention, the average carbon number is preferably 20 to 35, more preferably 25 to 35, and still more preferably 28 to 30.

Further, the% C _p of the lubricating base oil of the present invention is not particularly limited, but is preferably 80 or more, more preferably 82 to 99, still more preferably 85 to 98, and still more preferably 90 to 97. If the% C _p of the lubricating base oil is less than 80, the viscosity-temperature characteristics, thermal / oxidative stability, and friction characteristics tend to be reduced, and when the additive is added to the lubricating base oil The effectiveness of the additive tends to decrease. Further, when the% C _p value of the lubricating base oil exceeds 99, the additive solubility will tend to be lower.

Although% _{C N} of the lubricating base oil of the present invention is not particularly limited, preferably 12 or less, more preferably 1 to 12, more preferably from 3 to 10. If the% C _N value of the lubricating base oil exceeds 12, the viscosity - temperature characteristic, heat and oxidation stability and frictional properties will tend to be reduced. Moreover, when% _CN is less than 1, the solubility of the additive tends to decrease.

Although% _{C A} of the lubricating base oil of the present invention is not particularly limited, preferably 0.7 or less, more preferably 0.6 or less, more preferably 0.1 to 0.5 or less. When% C _A of the lubricating base oil exceeds 0.7, the viscosity - temperature characteristic, heat and oxidation stability and frictional properties will tend to be reduced. Moreover,% C _A of the lubricating base oil of the invention may be 0% by 0.1 or more C _A, it is possible to further increase the solubility of additives.

Further, it the ratio of the percentages in the lubricating base oil C _P and% C _N of the present invention is not particularly limited,% preferably C P _/% C _N is 7 or more, and 7.5 or more More preferably, it is 8 or more. When% C _P /% _CN is less than 7, viscosity-temperature characteristics, thermal / oxidative stability and friction characteristics tend to be reduced, and further when an additive is blended in the lubricating base oil. The effectiveness of the additive tends to decrease. _{Moreover,% C} P /% C _N is preferably 200 or less, more preferably 100 or less, more preferably 50 or less, particularly preferably 25 or less. By setting% C _P /% _CN to 200 or less, the solubility of the additive can be further increased.

Incidentally, _say% C P in the present invention,% _C A _N and% _{C A,} obtained by a method in accordance with ASTM D 3238-85, respectively (n-d-M ring analysis), the total carbon number of the paraffin carbon number The percentage of the total number of naphthene carbons to the total number of carbons, and the percentage of the total number of aromatic carbons to the total number of carbons. That is, the preferred ranges of% C _P ,% C _N and% C _A described above are based on the values obtained by the above method. For example, even a lubricating base oil containing no naphthene is obtained by the above method. is% C _N may indicate a value greater than zero.

  Further, the sulfur content in the lubricating base oil of the present invention depends on the sulfur content of the raw material. For example, when a raw material that does not substantially contain sulfur such as a synthetic wax component obtained by a Fischer-Tropsch reaction or the like is used, a lubricating base oil that does not substantially contain sulfur can be obtained. In addition, when using raw materials containing sulfur such as slack wax obtained in the refining process of the lubricating base oil and microwax obtained in the refining process, the sulfur content in the obtained lubricating base oil is usually 100 mass ppm. That's it. In the lubricating base oil of the present invention, the content of sulfur is preferably 100 mass ppm or less, more preferably 50 mass ppm or less, from the viewpoint of further improving thermal and oxidation stability and reducing sulfur content. Is more preferably 10 ppm by mass or less, and particularly preferably 5 ppm by mass or less.

  Further, from the viewpoint of cost reduction, it is preferable to use slack wax or the like as a raw material. In that case, the sulfur content in the obtained lubricating base oil is preferably 50 ppm by mass or less, and preferably 10 ppm by mass or less. More preferred. In addition, the sulfur content as used in the field of this invention means the sulfur content measured based on JISK2541-1996.

  Further, the nitrogen content in the lubricating base oil of the present invention is not particularly limited, but is preferably 5 ppm by mass or less, more preferably 3 ppm by mass or less, and further preferably 1 ppm by mass or less. If the nitrogen content exceeds 5 ppm by mass, the thermal and oxidation stability tends to decrease. In addition, the nitrogen content as used in the field of this invention means the nitrogen content measured based on JISK2609-1990.

The kinematic viscosity at 100 ° C. of the lubricating base oil of the present invention is not particularly limited and is usually 1 to 10 mm ² / s, preferably 3.5 to ⁶ mm ² / s, more preferably 3.7 to 4.5 mm ² / s, more preferably from 3.9~4.2mm ² / s. When the kinematic viscosity at 100 ° C. of the lubricating base oil is less than 3.5 mm ² / s, the evaporation loss tends to increase, and when it exceeds 6 mm ² / s, the low-temperature viscosity characteristics at −40 ° C. are greatly increased. It tends to get worse.

Further, the kinematic viscosity at 40 ° C. of the lubricating base oil of the present invention is not particularly limited and is usually 5 to 100 mm ² / s, preferably 12 to 32 mm ² / s, more preferably 13 to 19 mm ² / s. More preferably, it is 15-17.5 mm < ² > / s. When the kinematic viscosity at 40 ° C. of the lubricating base oil is less than 12 mm ² / s, the evaporation loss tends to increase, and when it exceeds 32 mm ² / s, the low-temperature viscosity characteristics at −40 ° C. tend to deteriorate. is there.

  The freezing point of the lubricating base oil of the present invention is not particularly limited, but is preferably −20 ° C. or lower, more preferably −25 ° C. or lower, and further preferably −28 ° C. or lower. In addition, under the temperature condition of about −30 ° C., sufficient low temperature characteristics may be obtained even when the freezing point of the lubricating base oil exceeds −25 ° C., but the low temperature viscosity at −35 ° C. or lower. In order to realize a lubricating oil excellent in characteristics (CCS viscosity, MRV viscosity, BF viscosity), particularly a lubricating oil having a greatly improved MRV viscosity at −40 ° C., it is important that the freezing point is −20 ° C. or lower. Yes, it is preferably -25 ° C or lower. In addition, the low temperature performance can be improved by lowering the freezing point of the lubricating base oil, but from the viewpoint of lowering the viscosity index and economy, the freezing point is preferably −45 ° C. or higher, more preferably −40 ° C. or higher. Preferably it is -35 degreeC or more. In the present invention, by setting the freezing point of the lubricating base oil to −35 to −25 ° C., a high-viscosity index and low temperature characteristics can be achieved at a higher level, and a lubricating base oil excellent in economy is obtained. It is particularly preferable because it can be used. Here, the lubricating base oil having a freezing point of −20 ° C. or less can be obtained by performing a dewaxing process such as the solvent dewaxing method or the contact dewaxing method described above. Any dewaxing treatment method may be adopted as long as the freezing point can be set to -20 ° C or lower.

  In addition, the freezing point as used in the field of this invention observes the flow of the sample measured by setting the pour point measurement interval (2.5 degreeC) in JISK2269-1987 (JIS method pour point) to 1 degreeC. It means a temperature 1 ° C. lower than the minimum temperature. In addition, although the result of a 2.5 degreeC space | interval is obtained in the JIS method pour point, in consideration of the measurement error and the reproduction accuracy of this method, it is not appropriate in the present invention in which the critical point of the low temperature characteristic is strictly controlled.

  The CCS viscosity of the lubricating base oil of the present invention at −35 ° C. is preferably 2800 mPa · s or less, more preferably 2200 mPa · s or less, and still more preferably 2000 mPa · s or less. In addition, the CCS viscosity at −35 ° C. in the present invention means a viscosity measured in accordance with JIS K2010-1993.

  Further, in the lubricating oil composition of the present invention, by containing the lubricating base oil of the present invention, the MRV viscosity at −40 ° C. is preferably 30000 mPa · s or less, more preferably 20000 mPa · s or less, and still more preferably. 15000 mPa · s or less, even more preferably 13000 mPa · s or less, more preferably 12000 mPa · s or less, particularly preferably 10000 mPa · s or less, and most preferably 8000 mPa · s or less, and the yield stress is also 0 Pa (yield). No stress). The MRV viscosity and yield stress at −40 ° C. in the present invention mean the viscosity and yield stress measured in accordance with ASTM D 4684, respectively.

  Furthermore, in the lubricating oil composition of the present invention, by containing the lubricating base oil of the present invention, the BF viscosity at −40 ° C. is preferably 20000 mPa · s or less, more preferably 15000 mPa · s or less, and even more preferably. Can be 10000 mPa · s or less, particularly preferably 8000 mPa · s or less. In addition, the BF viscosity at −40 ° C. in the present invention means a viscosity measured according to JPI-5S-26-99.

Moreover, it is preferable that the lubricating base oil of the present invention satisfies the condition represented by the following formula (1). 1.435 ≦ n ₂₀ −0.002 × kv100 ≦ 1.453 (1)
[Wherein n ₂₀ represents the refractive index of the lubricating base oil at 20 ° C., and kv100 represents the kinematic viscosity (mm ² / s) of the lubricating base oil at 100 ° C. ]

Furthermore, n ₂₀ −0.002 × kv100 in the lubricating base oil of the present invention is preferably 1.435 to 1.450, more preferably 1.440 to 1.449, and still more preferably 1.442 to 1.40. 448, particularly preferably 1.444 to 1.447. In order to produce a lubricating base oil having such properties, a raw material mainly composed of the aforementioned synthetic wax and / or slack wax is used as a raw material to be introduced into the hydrocracking and / or hydroisomerization process. It is preferable to use a raw material mainly composed of the aforementioned synthetic wax and / or slack wax A. In this case, the proportion of the branched paraffin in the lubricating base oil is preferably 80 to 99% by mass. In the case of the lubricating base oil obtained using the synthetic wax as a raw material, the lubricating base The proportion of the branched paraffin in the oil is more preferably 95 to 99% by mass, and still more preferably 97 to 99% by mass. In the case of the lubricating base oil obtained using the slack wax A as a raw material, the branched paraffin is used. The ratio is more preferably 82 to 98% by mass, and still more preferably 90 to 95% by mass.

Further, the lubricating base oil of the present invention contains 90% by mass or more of the saturated component, and the proportion of the cyclic saturated component in the saturated component is 5 to 40% by mass, preferably 10 to 25% by mass. In the case of oil, n ₂₀ −0.002 × kv100 is 1.435 to 1.453, preferably 1.440 to 1.452, more preferably 1.442 to 1.451, and still more preferably 1. .444 to 1.450. In order to produce a lubricating base oil having such properties, a raw material mainly composed of the aforementioned synthetic wax and / or slack wax is used as a raw material to be introduced into the hydrocracking and / or hydroisomerization process. It is preferable to use a raw material mainly composed of the aforementioned slack wax B. In this case, the proportion of the branched paraffin in the lubricating base oil is more preferably 54 to 99% by mass, further preferably 58 to 95% by mass, still more preferably 70 to 92% by mass, and particularly preferably. 80 to 90% by mass.

_By setting n ₂₀ -0.002 × kv100 within the above range, viscosity-temperature characteristics and thermal / oxidation stability can be achieved at a higher level, and an additive is added to the lubricating base oil. In this case, the function of the additive can be expressed at a higher level while the additive is sufficiently and stably dissolved and held in the lubricating base oil. Furthermore, by setting n ₂₀ −0.002 × kv100 within the above range, the friction characteristics of the lubricating base oil itself can be improved, and as a result, an improvement in friction reduction effect and an improvement in energy saving can be achieved. can do.

When n ₂₀ −0.002 × kv100 exceeds the upper limit, the viscosity-temperature characteristics, thermal / oxidation stability, and friction characteristics become insufficient, and further, an additive is blended in the lubricating base oil. In some cases, the effectiveness of the additive tends to decrease. Further, when n ₂₀ −0.002 × kv100 is less than the lower limit, when an additive is blended in the lubricating base oil, the solubility of the additive becomes insufficient, and the lubricating base oil contains Since the effective amount of the additive that is dissolved and held is lowered, the function of the additive tends to be unable to be obtained effectively.

In addition, the refractive index at 20 ° C. of the lubricating base oil of the present invention is preferably 1.450 to 1.465, more preferably 1.452 to 1.463, and even more preferably 1 in order to satisfy the above formula. .453 to 1.462. In addition, the refractive index (n20) in ₂₀ degreeC said by this invention means the refractive index measured in 20 degreeC based on ASTMD1218-92. The kinematic viscosity (kv100) at 100 ° C. in the present invention means a kinematic viscosity measured at 100 ° C. in accordance with JIS K 2283-1993.

  The pour point of the lubricating base oil of the present invention is preferably −20 ° C. or lower, more preferably −22.5 ° C. or lower, still more preferably −25 ° C. or lower, even more preferably −27.5 ° C. or lower, particularly Preferably it is -30 degrees C or less. When the pour point exceeds the upper limit, the low temperature viscosity characteristics at −35 ° C. or lower of the lubricating base oil and the lubricating oil composition tend to be lowered. In addition, the pour point as used in the field of this invention means the pour point measured based on JISK2269-1987.

Further, the density (ρ ₁₅ , unit: g / cm ³ ) of the lubricating base oil of the present invention at 15 ° C. is preferably 0.835 g / cm ³ or less, more preferably 0.830 g / cm ³ or less, still more preferably. Is 0.825 g / cm ³ or less, and preferably 0.810 g / cm ³ or more. In addition, the density in 15 degreeC said by this invention means the density measured in 15 degreeC based on JISK2249-1995.

  The NOACK evaporation amount of the lubricating base oil of the present invention is not particularly limited, but is preferably 20% by mass or less, more preferably 16% by mass or less, still more preferably 15% by mass or less, and still more preferably 14% by mass or less. Especially preferably, it is 12 mass% or less, Preferably it is 6 mass% or more, More preferably, it is 8 mass% or more, More preferably, it is 10 mass% or more. When the NOACK evaporation amount is the lower limit value, it tends to be difficult to improve the low temperature viscosity characteristics. Further, when the NOACK evaporation amount exceeds the upper limit value, when the lubricating base oil is used as the lubricating oil for an internal combustion engine, the evaporation loss amount of the lubricating oil increases, and accordingly, catalyst poisoning is promoted. Therefore, it is not preferable. In addition, the NOACK evaporation amount as used in the field of this invention means the evaporation loss amount measured based on ASTM D 5800-95.

  Further, the iodine value of the lubricating base oil of the present invention is preferably 2.5 or less, more preferably 1.5 or less, still more preferably 1 or less, particularly preferably 0.8 or less, and 0.01 However, it is preferably 0.01 or more, more preferably 0.1 or more, and still more preferably 0.5 or more, from the viewpoint of a small effect that is commensurate with it and economic efficiency. By setting the iodine value of the lubricating base oil to 2.5 or less, the thermal and oxidation stability can be dramatically improved. The “iodine value” in the present invention means an iodine value measured by an indicator titration method of JIS K 0070 “acid value, saponification value, iodine value, hydroxyl value, and unsaponification value of a chemical product”. .

  In addition, regarding the distillation properties of the lubricating base oil of the present invention, the initial boiling point (IBP) is preferably 300 to 380 ° C., more preferably 320 to 370 ° C., still more preferably 330 to 360 ° C. in gas chromatography distillation. It is. Moreover, 10% distillation temperature (T10) becomes like this. Preferably it is 340-420 degreeC, More preferably, it is 350-410 degreeC, More preferably, it is 360-400 degreeC. Moreover, 50% distillation temperature (T50) becomes like this. Preferably it is 380-460 degreeC, More preferably, it is 390-450 degreeC, More preferably, it is 400-460 degreeC. Moreover, 90% distillation temperature (T90) becomes like this. Preferably it is 440-500 degreeC, More preferably, it is 450-490 degreeC, More preferably, it is 460-480 degreeC. Moreover, an end point (FBP) becomes like this. Preferably it is 460-540 degreeC, More preferably, it is 470-530 degreeC, More preferably, it is 480-520 degreeC. Moreover, T90-T10 becomes like this. Preferably it is 50-100 degreeC, More preferably, it is 60-95 degreeC, More preferably, it is 80-90 degreeC. Moreover, FBP-IBP becomes like this. Preferably it is 100-250 degreeC, More preferably, it is 120-180 degreeC, More preferably, it is 130-160 degreeC. Moreover, T10-IBP becomes like this. Preferably it is 10-70 degreeC, More preferably, it is 15-60 degreeC, More preferably, it is 20-50 degreeC. Moreover, FBP-T90 becomes like this. Preferably it is 10-50 degreeC, More preferably, it is 20-40 degreeC, More preferably, it is 25-35 degreeC. By setting IBP, T10, T50, T90, FBP, T90-T10, FBP-IBP, T10-IBP, and FBP-T90 to the above preferred ranges, further improvement in low-temperature viscosity and further reduction in evaporation loss Is possible. In addition, about each of T90-T10, FBP-IBP, T10-IBP, and FBP-T90, when the distillation range is made too narrow, the yield of lubricating base oil is deteriorated, which is not preferable in terms of economy. . In the present invention, IBP, T10, T50, T90 and FBP mean distillate points measured in accordance with ASTM D 2887-97, respectively.

  Moreover, although the residual metal content in the lubricating base oil of the present invention is derived from the metal content contained in the catalyst and raw materials which are inevitably mixed in the production process, it is preferable that the residual metal content is sufficiently removed. For example, the contents of Al, Mo, and Ni are each preferably 1 mass ppm or less. If the content of these metals exceeds the above upper limit, the function of the additive blended with the lubricating base oil tends to be inhibited.

  In addition, the residual metal content as used in the field of this invention means the metal content measured based on JPI-5S-38-2003.

  Further, according to the lubricating base oil of the present invention, the content of the saturated component, the proportion of the cyclic saturated component in the saturated component, the viscosity index, the aniline point, and the proportion of ε-methylene satisfy the above conditions, so that excellent heat Although oxidation stability can be achieved, the RBOT life is preferably 350 min or more, more preferably 370 min or more, and further preferably 380 min or more. When the RBOT life is less than the lower limit, the viscosity-temperature characteristics and thermal / oxidative stability of the lubricating base oil tend to decrease. Further, when an additive is blended in the lubricating base oil, The effectiveness of the additive tends to decrease.

  The RBOT life as used herein refers to a composition in which 0.2% by mass of a phenolic antioxidant (2,6-di-tert-butyl-p-cresol; DBPC) is added to a lubricating base oil. It means the RBOT value measured according to JIS K 2514-1996.

  Although the lubricating base oil of the present invention can be used alone as a lubricating oil, the lubricating base oil of the present invention is used in combination with one or more other base oils and / or additives. It may be used as a composition.

  When the lubricating oil composition of the present invention contains the lubricating base oil of the present invention and another base oil, the proportion of the lubricating base oil of the present invention in the mixed base oil is 30% by mass. Preferably, the content is 50% by mass or more, and more preferably 70% by mass or more.

Although it does not restrict | limit especially as another base oil used together with the lubricating base oil of this invention, As mineral base oil, for example, solvent refined mineral oil whose kinematic viscosity in 100 degreeC is 1-100 mm < ² > / s, hydrogenation Cracked mineral oil, hydrorefined mineral oil, solvent dewaxing base oil and the like.

  Synthetic base oils include poly α-olefins or hydrides thereof, isobutene oligomers or hydrides thereof, isoparaffins, alkylbenzenes, alkylnaphthalenes, diesters (ditridecyl glutarate, di-2-ethylhexyl adipate, diisodecyl adipate, ditridec Decyl adipate, di-2-ethylhexyl sebacate, etc.), polyol ester (trimethylolpropane caprylate, trimethylolpropane pelargonate, pentaerythritol 2-ethylhexanoate, pentaerythritol pelargonate, etc.), polyoxyalkylene glycol, dialkyl Examples thereof include diphenyl ether and polyphenyl ether, and among them, poly α-olefin is preferable. As the poly α-olefin, typically, an oligomer or co-oligomer (1-octene oligomer, decene oligomer, ethylene-propylene co-oligomer, etc.) having 2 to 32 carbon atoms, preferably 6 to 16 carbon atoms, and those. Of the hydrides.

  The production method of the poly-α-olefin is not particularly limited. For example, Friedel-Crafts catalyst containing a complex of aluminum trichloride or boron trifluoride with water, alcohol (ethanol, propanol, butanol, etc.), carboxylic acid or ester. And a method of polymerizing α-olefin in the presence of a polymerization catalyst such as

  In addition, the lubricating oil composition of the present invention can further contain an additive. The additive contained in the lubricating oil composition of the present invention is not particularly limited, and any additive conventionally used in the field of lubricating oil can be used. Specific examples of such lubricating oil additives include antioxidants, ashless dispersants, metallic detergents, extreme pressure agents, antiwear agents, viscosity index improvers, pour point depressants, friction modifiers, oiliness agents. , Corrosion inhibitors, rust inhibitors, demulsifiers, metal deactivators, seal swelling agents, antifoaming agents, colorants and the like. These additives may be used individually by 1 type, and may be used in combination of 2 or more type.

  The lubricating oil composition of the present invention preferably contains a pour point depressant and / or a viscosity index improver among the above-mentioned additives from the viewpoint that the BF viscosity and MRV viscosity at −40 ° C. or lower can be greatly improved. . The pour point of the lubricating oil composition containing the pour point depressant and / or viscosity index improver is preferably −60 to −35 ° C., and more preferably −50 to −40 ° C.

  Moreover, it is preferable that the lubricating oil composition of this invention contains a viscosity index improver from the point which can further improve a viscosity-temperature characteristic. Viscosity index improvers include non-dispersed or dispersed polymethacrylates, dispersed ethylene-α-olefin copolymers or hydrides thereof, polybutylene or hydrides thereof, styrene-diene hydrogenated copolymers, styrene-anhydrous Maleic acid ester copolymers, polyalkylstyrenes and the like are mentioned, among which the weight average molecular weight is 10,000 to 1,000,000, preferably 100,000 to 900,000, more preferably 150,000 to 500,000. More preferably, a non-dispersion type viscosity index improver and / or a dispersion type viscosity index improver of 180,000 to 400,000 is preferably used. The PSSI (Permanent Shear Stability Index) of the viscosity index improver is not particularly limited, but is preferably 1 to 100, more preferably 10 to 90, and more preferably 50 or more in order to further improve fuel economy performance. Particularly preferably, it is desirable to set it to 55 or more. In order to achieve both high levels of shear stability and fuel saving performance, it is preferably 25 to 50, more preferably 30 to 45. It is to be noted that the PSSI referred to here, ASTM D 6022-01 (Standard Practice for Calculation of Permanent Shear Stability Index) to comply, ASTM D 6278-02 (Test Method for Shear Stability of Polymer Containing Fluid Using a European Diesel Injector Apparatus ) Is the permanent shear stability index of the polymer, calculated based on

  Furthermore, among the above-mentioned viscosity index improvers, polymethacrylate-based viscosity index improvers are preferable because they are excellent in low-temperature fluidity, and in particular, dispersible polymethacrylate-based viscosity index, because they also have dispersibility of oxidative degradation products. An improver is preferred.

  The content of the viscosity index improver in the lubricating oil composition of the present invention is preferably 0.1 to 15% by mass, more preferably 0.5 to 5% by mass, based on the total amount of the composition. When the content of the viscosity index improver is less than 0.1% by mass, the effect of improving the viscosity-temperature characteristics due to its addition tends to be insufficient, and when it exceeds 15% by mass, the thermal / oxidative stability is increased. It tends to decrease.

The kinematic viscosity at 100 ° C. of the lubricating oil composition of the present invention is not particularly limited, but is preferably 4.5 to 21.9 mm ² / s, more preferably 5 to 16.3 mm ² / s, and still more preferably 5.5. ˜12.5 mm ² / s, particularly preferably 5.5 to 9.3 mm ² / s. The viscosity index is not particularly limited, but is preferably 160 or more, more preferably 180 or more, still more preferably 200 or more, still more preferably 210 or more, and particularly preferably 220 or more. By increasing the viscosity index of the lubricating oil composition, it is possible to obtain a lubricating oil composition having an excellent viscosity index from a low temperature of −35 ° C. or lower to a high temperature, and further improve the energy saving (fuel saving performance), in particular, Engine oil and drive transmission lubricating oil can be obtained. In the present invention, to obtain a kinematic viscosity at 100 ° C. and fuel-saving engine oil 0 W-10 or 0 W-20 of 5 to 9 mm ² / s, the fuel-saving driving transmission device for lubricating oil 5 to 6 mm ² / s, etc. be able to.

  The lubricating base oil and lubricating oil composition of the present invention having the above-described structure are excellent in viscosity-temperature characteristics and thermal / oxidative stability, and improved in friction characteristics of the lubricating base oil itself, thereby reducing friction. It is possible to achieve an improvement in effect and, in turn, an improvement in energy saving. In addition, in the lubricating oil composition of the present invention, when an additive is blended in addition to the lubricating base oil of the present invention, the function of the additive (the effect of improving the heat and oxidation stability by the antioxidant, friction adjustment) The friction reducing effect by the agent and the wear resistance improving effect by the antiwear agent can be expressed at a higher level. Therefore, the lubricating base oil and lubricating oil composition of the present invention can be suitably used in various lubricating oil fields. Specific uses of the lubricating base oil and lubricating oil composition of the present invention include passenger car gasoline engines, motorcycle gasoline engines, diesel engines, gas engines, gas heat pump engines, marine engines, power generation engines, etc. Used in internal combustion engines (lubricating oil for internal combustion engines), automatic transmissions, manual transmissions, continuously variable transmissions, final reduction gears, etc. Hydraulic fluids used in hydraulic equipment for compressors, construction machinery, etc., compressor oil, turbine oil, industrial gear oil, refrigeration oil, rust prevention oil, heat medium oil, gas holder seal oil, bearing oil, paper machine oil, Examples include machine tool oil, sliding guide surface oil, electrical insulating oil, cutting oil, press oil, rolling oil, heat treatment oil, etc., and the lubricating base oil and lubricating oil composition of the present invention are used for these applications. By improving the viscosity-temperature characteristics, thermal / oxidation stability, energy savings, fuel economy, etc. of each lubricating oil, the service life of each lubricating oil and the reduction of environmentally hazardous substances can be achieved at a high level. Will be able to.

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

[Example 1]
800 g of USY zeolite and 200 g of an alumina binder were mixed and kneaded and molded into a cylindrical shape having a diameter of 1/16 inch (about 1.6 mm) and a height of 6 mm. The obtained molded body was fired at 450 ° C. for 3 hours to obtain a carrier. By impregnating this carrier with an aqueous solution of dichlorotetraamineplatinum (II) in an amount of 0.8% by mass in terms of platinum, drying at 120 ° C. for 3 hours, and baking at 400 ° C. for 1 hour, The desired catalyst was obtained.

Next, 200 ml of the obtained catalyst was charged into a fixed-type flow reactor, and hydrocracking / hydroisomerization of a feedstock oil containing paraffinic hydrocarbons was performed using this reactor. In this step, FT wax (hereinafter referred to as “WAX1”) having a paraffin content of 95% by mass and having a carbon number distribution of 20 to 80 was used as the raw material oil. Table 1 shows the properties of WAX1. The hydrocracking conditions were a hydrogen pressure of 3 MPa, a reaction temperature of 350 ° C., LHSV 2.0 h ^−1, and a fraction (decomposition product) having a boiling point of 380 ° C. or lower with respect to the raw material was 30% by mass (decomposition rate 30%). A cracking / isomerization product oil was obtained.

Next, the decomposition product obtained by the above hydrocracking was distilled under reduced pressure to obtain a lubricating oil fraction having a kinematic viscosity at 100 ° C. of 4 mm ² / s. The lubricating oil fraction was subjected to solvent dewaxing using a methyl ethyl ketone-toluene mixed solvent, the solvent / oil ratio was quadrupled, and the resulting solvent dewaxed oil had a freezing point of -25 ° C. or less. No. 1 lubricating base oil (hereinafter referred to as “base oil 1”) was obtained. The dewaxing temperature at this time was −25 ° C.

[Example 2]
The fraction separated by vacuum distillation in the step of refining the solvent refined base oil was subjected to hydrogenation after solvent extraction with furfural and then dewaxed with a methyl ethyl ketone-toluene mixed solvent. The wax obtained by further deoiling the slack wax removed during the solvent dewaxing (hereinafter referred to as “WAX2”) was used as a raw material for the lubricating base oil. Table 2 shows the properties of WAX2.

Next, hydrocracking of WAX2 was performed in the presence of a hydrocracking catalyst under the conditions of a hydrogen partial pressure of 5 MPa, an average reaction temperature of 350 ° C., and LHSV1hr ⁻¹ . As the hydrocracking catalyst, a catalyst in which 3% by mass of nickel and 15% by mass of molybdenum were supported on an amorphous silica / alumina carrier (silica: alumina = 20: 80 (mass ratio)) was used in a sulfurized state.

Next, the decomposition product obtained by the above hydrocracking was distilled under reduced pressure to obtain a lubricating oil fraction having a kinematic viscosity at 100 ° C. of 4 mm ² / s. The lubricating oil fraction was subjected to solvent dewaxing using a methyl ethyl ketone-toluene mixed solvent, the solvent / oil ratio was quadrupled, and the resulting solvent dewaxed oil had a freezing point of -25 ° C. or less. No. 2 lubricating base oil (hereinafter referred to as “base oil 2”) was obtained. The dewaxing temperature at this time was −32 ° C.

  Table 3 shows various properties and performance evaluation test results for the lubricating base oils of Examples 1 and 2. In addition, as Comparative Examples 1 to 4, various properties and performance evaluation test results for base oils 3 to 6 which are conventional high viscosity index base oils are shown in Table 4.

  From the results shown in Tables 3 and 4, the lubricating base oils of Examples 1 and 2 are superior in low temperature viscosity characteristics (CCS viscosity at −35 ° C.) as compared with the lubricating base oils of Comparative Examples 1 to 4. You can see that The base oil 3 and the base oil 4 are lubricating base oils produced in the same manner as the base oil 2 except that the above-mentioned WAX2 was used as a raw material and the solvent was removed at -20 to -23 ° C. Except for the proportion of methylene exceeding 20% (20 to 24%), the constituent requirements of claim 1 of the present application are satisfied and the properties are substantially the same as those of base oil 2 or base oil 1, but the viscosity index is 140 to 140. The CCS viscosity at −35 ° C. is sufficiently high as 150 and less than 3000 mPa · s (2200 to 2900 mPa · s).

[Examples 3 and 4, Comparative Examples 5 to 8]
In Examples 3 and 4 and Comparative Examples 5 to 8, the above base oils 1 to 6 and the dispersion type polymethacrylate having PSSI of 40 and performance additives (antioxidant, ashless dispersant, metallic detergent, abrasion) Including lubricants, etc.), lubricating oil compositions having the compositions shown in Tables 5 and 6 were prepared. Various properties of the resulting lubricating oil composition are shown in Tables 5 and 6.

[NOx absorption test]
For each of the lubricating oil compositions of Examples 3 and 4 and Comparative Examples 5 to 8, a NOx absorption test was performed as follows. The change with time of the acid value was measured when NOx-containing gas was blown into the test oil and forcedly deteriorated by a method in accordance with 1992, 10, 465 of the Japanese Tribology Conference Proceedings. The test temperature in this test was 140 ° C., and the NOx concentration in the NOx-containing gas was 1200 ppm. The O ₂ concentration was 85%. Tables 5 and 6 show the increase in acid value after 144 hours from the start of blowing NOx gas. In the table, the smaller the increase in the acid value, the longer the drain oil that can be used for a longer time even in the presence of NOx used in an internal combustion engine.

From the results shown in Tables 5 and 6, the lubricating oil compositions of Comparative Examples 5 and 6 have a sufficiently low temperature performance of MRV viscosity at −40 ° C. of 60000 mPa · s or less, and the lubricating oil compositions of Comparative Examples 7 and 8 The viscosity index is higher than that of products, and the increase in acid value in the presence of NOx is also small. However, it can be seen that the lubricating oil compositions of Examples 3 and 4 are superior in low-temperature viscosity characteristics (MRV viscosity at −40 ° C.) as compared with the lubricating oil compositions of Comparative Examples 5 to 8. Further, it can be seen that the lubricating oil compositions of Examples 3 and 4 have a higher viscosity index than the lubricating oil compositions of Comparative Examples 7 and 8, and are excellent in terms of thermal and oxidation stability.

Claims (3)

Contains 95% by weight or more of saturated components,
The ratio of the cyclic saturated component in the saturated component is 10% by mass or less,
The viscosity index is 110 or more,
An aniline point is 106 or more, and
A lubricating base oil characterized in that the proportion of ε-methylene in the total amount of constituent carbon is 14 to 20%.   The lubricating base oil according to claim 1 or 2, wherein the aromatic content is 5 mass% or less.   A lubricating oil composition comprising the lubricating base oil according to claim 1.