WO2018181431A1 - Grease composition and method for producing grease composition - Google Patents

Abstract

Provided is a grease composition including a base oil (A) and a thickener (B), wherein the thickener (B) includes a sodium salt (B1) represented by general formula (b-1). The grease composition can easily form a grease, has an appropriate worked penetration, and has a high dropping point. (In general formula (b-1), R1 each independently represents a substituted or unsubstituted C1 to 20 alkyl group, a substituted or unsubstituted C1 to 20 alkenyl group, or a substituted or unsubstituted C1 to 20 alkoxy group. n is an integer from 0 to 5. Additionally, when n is 2 or more and there are a plurality of R1s, the plurality of R1s may be the same or may differ from one another.)

Description

Grease composition and method for producing grease composition

The present invention relates to a grease composition and a method for producing the grease composition.

Grease is easier to seal than lubricating oil, and is widely used for lubrication of various sliding parts of automobiles and various industrial machines because the machine can be made smaller and lighter. Has been.
Although grease is mainly composed of a base oil and a thickener, the solid nature of the grease is imparted by the thickener, and the performance of the grease varies greatly depending on the thickener used.
Among them, greases using sodium salts as thickeners have been known for a long time and have been widely used for lubricating sliding parts provided in automobiles, electrical equipment, various industrial machines and the like.

For example, Patent Document 1 discloses a grease composition containing about 40% by mass of a sodium salt as a thickener together with a base oil.

US Patent 3,223,624

Generally, when sodium salt is used as a thickener, it is known that the sodium salt is difficult to be greased because it is difficult to form a fine fiber structure in the base oil.
Therefore, in order to make a grease when using a sodium salt as a thickener, the blending amount of the sodium salt as a thickener is about 40% by mass as in the grease composition disclosed in Patent Document 1, for example. It is a general finding that it is necessary to increase the amount of

Further, depending on various uses, in order to obtain a hard grease having a low miscibility by using sodium salt as a thickener, it is necessary to add a larger amount of sodium salt.
However, since the grease obtained by blending a large amount of sodium salt has a high solid content, a part of the sodium salt floats on the grease surface as particles larger than the oil film thickness, resulting in wear resistance. Detrimental effects such as lowering may occur. Further, when a large amount of sodium salt is added as a thickener, the base oil component in the obtained grease is insufficient, and there is a problem that the amount of wear of the members constituting the sliding portion and the like increases.
In addition, the grease using the sodium salt described in Patent Document 1 has a low dropping point and may not be suitable for use in a member that becomes high temperature.

The present invention has been made in view of the above problems, and an object of the present invention is to provide a grease composition that is easy to be greased, has an appropriate penetration, and has a high dropping point, and a method for producing the grease. And

The present inventor has found that a grease composition containing a sodium salt of an aromatic monocarboxylic acid having a specific structure as a thickener can solve the above problems, and has completed the present invention.

That is, the present invention provides the following [1] to [2].
[1] Contains a base oil (A) and a thickener (B),
A grease composition, wherein the thickener (B) comprises a sodium salt (B1) represented by the following general formula (b-1).

[In the general formula (b-1), each R ¹ independently represents an unsubstituted or substituted alkyl group having 1 to 20 carbon atoms or an unsubstituted or substituted alkenyl group having 1 to 20 carbon atoms. Represents an unsubstituted or substituted alkoxy group having 1 to 20 carbon atoms or a hydroxy group.
n is an integer of 0 to 5.
In the case where n is 2 or more R ¹ there are a plurality, the plurality of R ¹ may be the same or different from each other. ]

[2] A method for producing a grease composition, comprising the following step (1).
Step (1): A step of blending the base oil (A) with an aromatic monocarboxylic acid represented by the following general formula (bi) and sodium hydroxide.

[In the general formula (bi), each R ¹ independently represents an unsubstituted or substituted alkyl group having 1 to 20 carbon atoms, or an unsubstituted or substituted alkenyl group having 1 to 20 carbon atoms. Represents an unsubstituted or substituted alkoxy group having 1 to 20 carbon atoms or a hydroxy group.
n is an integer of 0 to 5.
In the case where n is 2 or more R ¹ there are a plurality, the plurality of R ¹ may be the same or different from each other. ]

The grease composition of the present invention is easily greased, has an appropriate blending consistency, and has a high dropping point.

The grease composition of the present invention contains a base oil (A) and a thickener (B).
Note that the grease composition of one embodiment of the present invention may further contain various additives used for general greases.

In the grease composition of one embodiment of the present invention, the total content of the base oil (A) and the thickener (B) is determined from the viewpoint of obtaining a grease composition having an appropriate blending degree and a high dropping point. The total amount (100% by mass) of the composition is preferably 70% by mass or more, more preferably 75% by mass or more, still more preferably 80% by mass or more, and still more preferably 85% by mass or more.
Hereinafter, details of each component contained in the grease composition of one embodiment of the present invention will be described.

<Base oil (A)>
The base oil (A) contained in the grease composition of the present invention may be one or more selected from mineral oil and synthetic oil.
As mineral oil, for example, atmospheric distillation residue oil obtained by atmospheric distillation of crude oil such as paraffinic crude oil, intermediate base crude oil, naphthenic crude oil, etc .; distillation obtained by vacuum distillation of the atmospheric distillation residual oil Oil; Mineral oil obtained by subjecting the distillate to one or more purification processes such as solvent deburring, solvent extraction, hydrocracking, solvent dewaxing, catalytic dewaxing, hydrorefining, etc .; Fischer-Tropsch from natural gas Examples thereof include mineral oil (GTL) obtained by isomerizing wax produced by a method or the like (GTL wax (Gas To Liquids WAX)).

Synthetic oils include, for example, α-olefin homopolymers or α-olefin copolymers (eg, α-olefin copolymers having 8 to 14 carbon atoms such as ethylene-α-olefin copolymers). Examples include hydrocarbon oils such as α-olefins and isoparaffins; alkylbenzenes; aromatic oils such as alkylnaphthalenes; ester oils such as polyol esters and dibasic acid esters; and ether oils such as polyalkylene glycols.

The kinematic viscosity at 40 ° C. of the base oil (A) used in one embodiment of the present invention is preferably 10 to 1500 mm ² / s, more preferably 25 to 1000 mm ² / s, more preferably 40 to 750 mm ^2. / S, more preferably 50 to 500 mm ² / s, still more preferably 60 to 350 mm ² / s.
The base oil (A) is a mixed base oil in which the kinematic viscosity is in the above range by combining two or more types of base oils having different kinematic viscosities, a high viscosity base oil and a low viscosity base oil. Also good.

The viscosity index of the base oil (A) used in one embodiment of the present invention is preferably 60 or more, more preferably 70 or more, still more preferably 80 or more, and still more preferably 100 or more.
In the present specification, the kinematic viscosity and the viscosity index mean values measured and calculated in accordance with JIS K2283: 2003.

In the grease composition of one embodiment of the present invention, the content of the base oil (A) is preferably 60 to 99.0% by mass, more preferably 70, based on the total amount (100% by mass) of the grease composition. To 95.0 mass%, more preferably 75 to 92.5 mass%, and still more preferably 80 to 90.0 mass%.

<Thickener (B)>
In the grease composition used in one aspect of the present invention, the content of the thickener (B) is such that the grease is easily formed into a grease, and from the viewpoint of obtaining a grease composition having an appropriate blending degree and a high dropping point. Based on the total amount (100% by mass) of the composition, it is preferably 1.0 to 30% by mass, more preferably 5.0 to 25% by mass, still more preferably 7.5 to 23% by mass, and still more preferably 10 to 20% by mass.

The thickener (B) contained in the grease composition of the present invention contains a sodium salt (B1) represented by the following general formula (b-1).

In the general formula (b-1), each R ¹ independently represents an unsubstituted or substituted alkyl group having 1 to 20 carbon atoms, an unsubstituted or substituted alkenyl group having 1 to 20 carbon atoms, It represents an unsubstituted or substituted alkoxy group having 1 to 20 carbon atoms or a hydroxy group.
n is an integer of 0 to 5.
In the case where n is 2 or more R ¹ there are a plurality, the plurality of R ¹ may be the same or different from each other.

For example, when only sodium salt of terephthalic acid or sodium salt of aliphatic carboxylic acid is used as a thickener, these sodium salts are difficult to form a fine fiber structure in the base oil. It is hard to become.
In addition, when a large amount of these sodium salts are blended to make a grease, the resulting grease has a high solid content, so that some of the sodium salt floats on the grease surface as particles larger than the oil film thickness. Thus, the grease composition is inferior in wear resistance.
On the other hand, the sodium salt (B1) contained as the thickener (B) in the grease composition of the present invention can form a finer fiber structure in the grease composition in the form of a mesh. Easy to grease.

The number of carbon atoms of the alkyl group, the alkenyl group, and the alkoxy group, which can be selected as R ¹ in the general formula (b-1), is easily greased, has an appropriate blending degree, and a high dropping point. From the viewpoint of obtaining a grease composition having the above, it is 1 to 20, preferably 1 to 12, more preferably 1 to 6, and further preferably 1 to 3.
Note that the carbon number does not include the carbon number of the substituent that the alkyl group, the alkenyl group, and the alkoxy group may have.

Examples of the alkyl group that can be selected as R ¹ include, for example, methyl group, ethyl group, n-propyl group, isopropyl group, n-butyl group, isobutyl group, s-butyl group, t-butyl group, pentyl group, Examples include hexyl group, heptyl group, octyl group, 2-ethylhexyl group, nonyl group, decyl group, undecyl group, dodecyl group, hexadecyl group, octadecyl group, and nonadecyl group.

The alkyl group may be a straight-chain alkyl group or a branched-chain alkyl group, but from the viewpoint of making a grease composition easy to grease and having an appropriate blending consistency and a high dropping point. A linear alkyl group is preferred.

The alkyl group that can be selected as R ¹ may have a substituent.
Examples of the substituent that the alkyl group may have include, for example, a cycloalkyl group, a vinyl group, an allyl group, an aryl group, an alkoxy group, a halogen group, a hydroxy group, an amino group, an imino group, a nitro group, and a silyl group. , And ester groups.
However, in one embodiment of the present invention, the alkyl group that can be selected as R ¹ is preferably an unsubstituted alkyl group.

Examples of the alkenyl group that can be selected as R ¹ include a vinyl group, propenyl group, butenyl group, pentenyl group, pentadienyl group, hexenyl group, hexadienyl group, heptenyl group, octenyl group, octadienyl group, 2-ethylhexenyl group, nonenyl group Group, decenyl group, undecenyl group, dodecenyl group, tridecenyl group, tetradecenyl group, pentadecenyl group, hexadecenyl group, heptadecenyl group, octadecenyl group, nonadecenyl group, eicocenyl group and the like.
The alkenyl group may be a linear alkenyl group or a branched alkenyl group, but is preferably a linear alkenyl group.

Also be selected as R ^1, alkenyl group may have a substituent.
Examples of the substituent that the alkenyl group may have include, for example, an alkyl group, a cycloalkyl group, an allyl group, an aryl group, an alkoxy group, a halogen group, a hydroxy group, an amino group, an imino group, a nitro group, and a silyl group. , And ester groups.
The alkyl group that can be selected as the substituent may be a linear alkyl group or a branched alkyl group, but is preferably a linear alkyl group.
Note that in one embodiment of the present invention, the alkenyl group that can be selected as R ¹ is preferably an unsubstituted alkenyl group.

R ¹ may be selected as the Examples of the alkoxy group include a methoxy group, an ethoxy group, n- propoxy group, isopropoxy group, n- butoxy group, isobutoxy group, s- butoxy group, t-butoxy group, pentyloxy Group, hexyloxy group, heptyloxy group, octyloxy group, 2-ethylhexyloxy group, nonyloxy group, decyloxy group, undecyloxy group, dodecyloxy group, hexadecyloxy group, octadecyloxy group, nonadecyloxy group, etc. .
The alkoxy group may be a linear alkoxy group or a branched alkoxy group, but is preferably a linear alkoxy group.

Further, the alkoxy group that can be selected as R ¹ may have a substituent.
Examples of the substituent that the alkoxy group may have include, for example, an alkyl group, a cycloalkyl group, a vinyl group, an allyl group, an aryl group, a halogen group, a hydroxy group, an amino group, an imino group, a nitro group, and a silyl group. , And ester groups.
The alkyl group that can be selected as the substituent may be a linear alkyl group or a branched alkyl group, but is preferably a linear alkyl group.
Incidentally, in one aspect of the present invention, may be selected as R ^1, the alkenyl group is preferably an unsubstituted alkenyl group.

Among these, R ¹ is an unsubstituted or substituted alkyl group having 1 to 20 carbon atoms from the viewpoint of making a grease composition having a suitable miscibility and a high dropping point as well as being easily greased. It is preferably an unsubstituted alkyl group having 1 to 20 carbon atoms.
Among the alkyl groups, a methyl group, an ethyl group, an n-propyl group, an isopropyl group, an n-butyl group, an isobutyl group, or an s-butyl group is preferable, and a methyl group, an ethyl group, or an n-group is preferable. A propyl group is more preferred, and a methyl group is still more preferred.

In the above general formula (b-1), n is an integer of 0 to 5, and is preferably 0 from the viewpoint of facilitating the formation of a grease and having a proper blending consistency and high dropping point. It is an integer of ˜4, more preferably an integer of 0 to 3, more preferably an integer of 0 to 2, and still more preferably 0 or 1.

Further, from the viewpoint of facilitating the formation of a grease and providing a grease composition having an appropriate blending consistency and high dropping point, the sodium salt (B1) is a sodium salt (B11) represented by the following general formula (b-11). And at least one selected from sodium salts (B12) represented by the following general formula (b-12).

In the above general formula (b-12), R ¹ is the same as the above general formula (b-1), and the same applies to preferred embodiments (group type, group carbon number, etc.).

In the grease composition of one aspect of the present invention, the sodium salt (B1) in the thickener (B1) is added from the viewpoint of facilitating the formation of a grease and having a moderate mixing consistency and a high dropping point. The content is preferably 5 to 100% by mass, more preferably 10 to 95% by mass, still more preferably 15 to 90% by mass, and still more preferably based on the total amount (100% by mass) of the thickener (B). 20 to 85% by mass.

<Sodium salt (B2)>
In the grease composition of one embodiment of the present invention, the thickener (B), together with the sodium salt (B1) described above, further contains the following general compounds from the viewpoint of obtaining a grease composition having an appropriate blending consistency and a high dropping point. It is preferable to include a sodium salt (B2) represented by the formula (b-2).

In the general formula (b-2), R ² represents an unsubstituted or substituted alkyl group having 7 to 22 carbon atoms or an unsubstituted or substituted alkenyl group having 7 to 22 carbon atoms.

By containing the sodium salt (B2) as the thickener (B), a finer fiber structure can be formed, so that it is easy to adjust the desired blending consistency. Moreover, it can be set as the grease composition which has a higher dropping point.
In addition, in the grease composition of this invention, since it contains the above-mentioned sodium salt (B1) as a thickener (B), it is easily prepared into grease. Furthermore, by containing the sodium salt (B2) represented by the above general formula, a grease composition having an appropriate blending consistency and a higher dropping point can be obtained.

The number of carbon atoms of the alkyl group and the alkenyl group that can be selected as R ² in the general formula (b-2) is 7 to 22, preferably 10 to 20, more preferably 12 to 19, More preferably, it is 15-19.
In addition, said carbon number may have the said alkyl group and the said alkenyl group, and carbon number of a substituent is not included.

Examples of the alkyl group that can be selected as R ² include a heptyl group, an octyl group, a 2-ethylhexyl group, a nonyl group, a decyl group, an undecyl group, a dodecyl group, a hexadecyl group, an octadecyl group, and a nonadecyl group. .
The alkyl group may be a linear alkyl group or a branched alkyl group, but is preferably a linear alkyl group.

The alkyl group that can be selected as R ² may have a substituent.
Examples of the substituent that the alkyl group may have include, for example, a cycloalkyl group, a vinyl group, an allyl group, an aryl group, an alkoxy group, a halogen group, an amino group, an imino group, a nitro group, a silyl group, and an ester. Groups and the like.
However, in one embodiment of the present invention, the alkyl group that can be selected as R ² is preferably an unsubstituted alkyl group.

Examples of the alkenyl group that can be selected as R ² include a heptenyl group, an octenyl group, an octadienyl group, a 2-ethylhexenyl group, a nonenyl group, a decenyl group, an undecenyl group, a dodecenyl group, a tridecenyl group, a tetradecenyl group, and a pentadecenyl group. , Hexadecenyl group, heptadecenyl group, octadecenyl group, nonadecenyl group, eicocenyl group and the like.
The alkenyl group may be a linear alkenyl group or a branched alkenyl group, but is preferably a linear alkenyl group.

The alkenyl group that can be selected as R ² may have a substituent.
Examples of the substituent that the alkenyl group may have include an alkyl group, a cycloalkyl group, an allyl group, an aryl group, an alkoxy group, a halogen group, an amino group, an imino group, a nitro group, a silyl group, and an ester. Groups and the like.
The alkyl group that can be selected as the substituent may be a linear alkyl group or a branched alkyl group, but is preferably a linear alkyl group.
Note that in one embodiment of the present invention, the alkenyl group that can be selected as R ² is preferably an unsubstituted alkenyl group.

Among these, R ² is preferably an unsubstituted or substituted alkyl group having 7 to 22 carbon atoms, and more preferably an unsubstituted alkyl group having 7 to 22 carbon atoms.
Among the alkyl groups, an undecyl group, a dodecyl group, a hexadecyl group, a heptadecyl group, an octadecyl group, or a nonadecyl group is preferable, and a dodecyl group, a hexadecyl group, a heptadecyl group, an octadecyl group, or a nonadecyl group. Is more preferred, and a heptadecyl group is even more preferred.

In the grease composition of one aspect of the present invention, the inclusion of sodium salt (B1) and sodium salt (B2) from the viewpoint of making the grease composition easy to be greased and having a proper blending consistency and high dropping point The quantity ratio [(B1) / (B2)] is a mass ratio, preferably 5/95 to 95/5, more preferably 10/90 to 90/10, still more preferably 15/85 to 85/15, and more. More preferably, it is 20/80 to 80/20, and particularly preferably 30/70 to 70/30.

In the grease composition of one embodiment of the present invention, the total content of the sodium salt (B1) and the sodium salt (B2) in the thickener (B) is preferably 60 based on the total amount of the thickener (B). To 100% by mass, more preferably 70 to 100% by mass, still more preferably 80 to 100% by mass, and still more preferably 90 to 100% by mass.

<Other thickeners>
The thickener (B) contained in the grease composition of one aspect of the present invention may be used in combination with a thickener other than sodium salts (B1) and (B2) as long as the effects of the present invention are not impaired. .

However, in the grease composition of one embodiment of the present invention, the content of the lithium atom-containing compound (β1) from the viewpoint of making the grease composition easy to be greased and having a proper blending consistency and a high dropping point, It is preferable to have as little as possible.
The content of the lithium atom-containing compound (β1) in the thickener (B) is preferably less than 5.0 mass%, more preferably 1 based on the total amount (100 mass%) of the thickener (B). Less than 0.0 mass%, more preferably less than 0.1 mass%.

From the same viewpoint as described above, the content of the metal salt (β2) of the aliphatic carboxylic acid having 2 to 7 carbon atoms is preferably as small as possible.
Examples of the metal atoms constituting the metal salt (β2) include alkali metal atoms such as sodium atoms and potassium atoms, alkaline earth metals such as calcium atoms, and aluminum.
The content of the metal salt (β2) in the thickener (B) is preferably less than 5.0 mass%, more preferably 1.0 mass%, based on the total amount (100 mass%) of the thickener. Less than, more preferably less than 0.1 mass.

<Various additives>
The grease composition of one embodiment of the present invention may further contain various additives used for general greases as long as the effects of the present invention are not impaired.
Examples of the various additives include extreme pressure agents, rust inhibitors, antioxidants, lubricity improvers, thickeners, modifiers, detergent dispersants, corrosion inhibitors, antifoaming agents, and metal deactivators. Etc.
These various additives may be used alone or in combination of two or more.

The content of each of the various additives in the grease composition of one embodiment of the present invention is appropriately set according to the type of the additive, and is preferably based on the total amount (100% by mass) of the grease composition. It is 0.01 to 20% by mass, more preferably 0.05 to 15% by mass, and still more preferably 0.1 to 10% by mass.

[Method for Producing Grease Composition of the Present Invention]
As a method for producing the above-described grease composition of the present invention, a known method can be applied, but from the viewpoint of obtaining an appropriate blending consistency and a high dropping point, a production method having at least the following step (1) is preferable, A production method having the following steps (1) to (3) is more preferred.
Step (1): A step of blending the base oil (A) with a carboxylic acid containing an aromatic monocarboxylic acid represented by the following general formula (bi) and sodium hydroxide.

In [the above general formula (b-i), R ¹ and n are the same as R ¹ and n in the general formula (b-1), preferred embodiments are also the same, as described above. ]
Step (2): A step of heating the solution obtained in step (1) while stirring to react the carboxylic acid with sodium hydroxide.
Step (3): A step of cooling the solution after step (2).

In the step (1), it is preferable to further blend an aliphatic monocarboxylic acid represented by the following general formula (b-ii) as the carboxylic acid.

[In general formula (b-ii) in, R ² is the same as R ² in the general formula (b-2), preferred embodiments are also the same, as described above. ]

In the step (1), a reaction product of the aromatic monocarboxylic acid represented by the general formula (bi) and sodium hydroxide becomes a sodium salt (B1) which is a thickener (B).
The reaction product of the aliphatic monocarboxylic acid represented by the general formula (b-ii) and sodium hydroxide becomes the sodium salt (B2) which is the thickener (B).
Therefore, each of the aromatic monocarboxylic acid, the aliphatic monocarboxylic acid, and sodium hydroxide so that the contents of the sodium salts (B1) and (B2) in the obtained grease composition are in the above ranges. The blending amount is prepared.

Sodium hydroxide is preferably added to a solution containing the base oil (A) and the carboxylic acid in the form of an aqueous solution dissolved in water.
And when sodium hydroxide is mix | blended with the form of aqueous solution, in order to evaporate and remove the water in a solution, it is preferable to heat up the solution after mixing the said aqueous solution to 100 degreeC or more.

In step (2), the reaction temperature is preferably 140 to 280 ° C, more preferably 150 to 250 ° C, and still more preferably 160 to 220 ° C.

In the step (3), during or after cooling, various additives for grease described above may be further blended and mixed.
The mixing temperature is preferably 140 ° C. or lower, more preferably 120 ° C. or lower, and still more preferably 90 ° C. or lower.

Further, in the step (3), it is preferable to perform a milling treatment on the grease composition, which is a reaction product after cooling, using a colloid mill, a roll mill or the like.

[Characteristics of the grease composition of the present invention]
The blending degree of the grease composition of one embodiment of the present invention at 25 ° C. is preferably 85 to 475, more preferably 115 from the viewpoint of setting the hardness of the grease composition in an appropriate range and improving wear resistance. 445 to 445, more preferably 130 to 430.
In addition, in this specification, a penetration degree means the value measured at 25 degreeC based on ASTMD217 method.

The dropping point of the grease composition of one embodiment of the present invention is preferably 200 ° C. or higher, more preferably 250 ° C. or higher, still more preferably 270 ° C. or higher, and still more preferably 290 ° C., from the viewpoint of improving high temperature characteristics. That's it.
In addition, in this specification, a dropping point means the value measured at 25 degreeC based on JISK2220 8: 2013.

[Use of grease composition of the present invention]
The mechanical component using the grease composition of the present invention is not particularly limited, and examples thereof include bearings and gears, and more specifically, various bearings such as slide bearings, rolling bearings, oil-impregnated bearings, fluid bearings, and gears. , Internal combustion engines, brakes, torque transmission parts, fluid joints, compression parts, chains, hydraulic parts, vacuum pump parts, clock parts, hard disk parts, refrigerator parts, cutting machine parts, Parts for rolling mills, parts for drawing and drawing machines, parts for rolling machines, parts for forging machines, parts for heat treatment machines, parts for heating media, parts for washing machines, parts for shock absorbers, parts for sealing devices, for construction machinery Examples include parts and parts for agricultural machinery.
Among these, it is preferable that the grease composition of the present invention is used for construction parts or agricultural machine parts.

Next, the present invention will be described in more detail with reference to examples, but the present invention is not limited to these examples. In addition, the measuring method of various physical-property values is as follows.

(1) Kinematic viscosity at 40 ° C., viscosity index Measured and calculated according to JIS K2283: 2003.
(2) Mixing penetration Measured at 25 ° C. according to ASTM D217 method.
(3) Dropping point Measured according to JIS K2220 8: 2013.

The mineral oil and carboxylic acid components used in the preparation of the grease compositions of the examples and comparative examples are as follows.
Mineral oil: Kinematic viscosity at 40 ° C. = 150 mm ² / s, viscosity index = 106.
Benzoic acid: an aromatic monocarboxylic acid in which n = 0 in the general formula (bi).
P-Toluic acid: an aromatic monocarboxylic acid in which n = 1 and R ¹ = methyl group in the general formula (bi).
-Terephthalic acid: aromatic dicarboxylic acid.
Stearic acid: An aliphatic monocarboxylic acid in which R ² = n-heptadecyl group (straight chain alkyl group having 17 carbon atoms) in the general formula (b-ii).

Examples 1 to 4 and Comparative Examples 1 to 2
To the 1 L separable flask, the carboxylic acid component of the type and blending amount shown in Table 1 was added to the mineral oil, the temperature was raised to 80 ° C. in an oil bath, and the carboxylic acid component was dissolved in the mineral oil.
And the sodium hydroxide aqueous solution of solid content concentration 45 mass% was added by the compounding quantity (active ingredient (solid content) conversion) shown in Table 1, and it heated to 100 degreeC, and water removed by evaporation.
After removing the water, the temperature was raised again by heating, and the reaction between the carboxylic acid component and sodium hydroxide was completed at 180 ° C.
After completion of the reaction, the reaction product was cooled to 25 ° C. and milled twice with a three roll.
As a result, grease compositions were obtained in Examples 1 to 4 and Comparative Example 2, but in Comparative Example 1, no grease was formed.
For the greased Examples 1 to 4 and Comparative Example 2, the penetration and dropping point were further measured. The measurement results are shown in Table 1.

From Table 1, the grease compositions of Examples 1 to 4 can be made into a grease even when the content of the thickener is a relatively small amount of 14% by mass, and the penetration degree is 200 to 350. A relatively hard grease was obtained. Also, the dropping point was high, and the heat resistance was excellent.
On the other hand, in Comparative Example 1, since it was not greased, the mixing penetration and the dropping point were not measured.
In addition, the grease composition of Comparative Example 2 had a penetration of 400 or more and was very soft, and the shape could not be maintained in the measurement container, so the dropping point could not be measured.

Claims (12)

1. Contains base oil (A) and thickener (B),
   A grease composition, wherein the thickener (B) comprises a sodium salt (B1) represented by the following general formula (b-1).
   

   

   
   [In the general formula (b-1), each R ¹ independently represents an unsubstituted or substituted alkyl group having 1 to 20 carbon atoms or an unsubstituted or substituted alkenyl group having 1 to 20 carbon atoms. Represents an unsubstituted or substituted alkoxy group having 1 to 20 carbon atoms or a hydroxy group.
   n is an integer of 0 to 5.
   In the case where n is 2 or more R ¹ there are a plurality, the plurality of R ¹ may be the same or different from each other. ]
2. The sodium salt (B1) is at least one selected from a sodium salt (B11) represented by the following general formula (b-11) and a sodium salt (B12) represented by the following general formula (b-12) The grease composition according to claim 1.
   

   

   
   [In the general formula (b-12), R ¹ is the same as defined in the general formula (b-1) described in claim 1. ]
3. The grease composition according to claim 1 or 2, wherein the content of the sodium salt (B1) in the thickener (B) is 5 to 100% by mass based on the total amount of the thickener (B).
4. The grease composition according to any one of claims 1 to 3, wherein the thickener (B) further comprises a sodium salt (B2) represented by the following general formula (b-2).
   

   

   
   [In the general formula (b-2), R ² represents an unsubstituted or substituted alkyl group having 7 to 22 carbon atoms, or an unsubstituted or substituted alkenyl group having 7 to 22 carbon atoms. . ]
5. The grease composition according to claim 4, wherein the content ratio [(B1) / (B2)] of the sodium salt (B1) and the sodium salt (B2) is 5/95 to 95/5 in terms of mass ratio. .
6. The total content of the sodium salt (B1) and the sodium salt (B2) in the thickener (B) is 60 to 100% by mass based on the total amount of the thickener (B). The grease composition as described.
7. The content of the lithium atom-containing compound (β1) in the thickener (B) is less than 5.0% by mass based on the total amount of the thickener (B). The grease composition described in 1.
8. The content of the metal salt (β2) of an aliphatic carboxylic acid having 2 to 7 carbon atoms in the thickener (B) is less than 5.0% by mass based on the total amount of the thickener (B). Item 8. The grease composition according to any one of Items 1 to 7.
9. The grease composition according to any one of claims 1 to 8, wherein the content of the thickener (B) is 1.0 to 30% by mass based on the total amount of the grease composition.
10. The grease composition according to any one of Claims 1 to 9, wherein the penetration at 25 ° C is 85 to 475.
11. The manufacturing method of a grease composition which has the following process (1).
    Step (1): A step of blending the base oil (A) with a carboxylic acid containing an aromatic monocarboxylic acid represented by the following general formula (bi) and sodium hydroxide.
    

    

    
    [In the general formula (bi), each R ¹ independently represents an unsubstituted or substituted alkyl group having 1 to 20 carbon atoms, or an unsubstituted or substituted alkenyl group having 1 to 20 carbon atoms. Represents an unsubstituted or substituted alkoxy group having 1 to 20 carbon atoms or a hydroxy group.
    n is an integer of 0 to 5.
    In the case where n is 2 or more R ¹ there are a plurality, the plurality of R ¹ may be the same or different from each other. ]
12. The method for producing a grease composition according to claim 11, wherein in step (1), an aliphatic monocarboxylic acid represented by the following general formula (b-ii) is further blended as the carboxylic acid.
    

    

    
    [In the general formula (b-ii), R ² represents an unsubstituted or substituted alkyl group having 7 to 22 carbon atoms, or an unsubstituted or substituted alkenyl group having 7 to 22 carbon atoms. . ]