JPS58122996A - Grease composition - Google Patents

Abstract

PURPOSE:A grease compsn. excellent in oxidation stability and having excellent performance for a rolling friction driving device, which is prepd. by using as the base oil a specified naphthenic hydrocarbon oil having three hydrogenated six-membered carbocyclic rings. CONSTITUTION:The titled grease compsn. is constituted of a consistency increasing agent such as calcium soap and a base oil of pour pt. <=0 deg.C, aniline pt. >=70 deg.C and traction factor >=0.08, substantially consisting of at least one 19-30C naphthenic hydrocarbon of formulaI(wherein R<1> is 1-3C alkylene; R<3-5> is 1-3C alkyl; l, m and n are each 0-3; x is 0 or 1) having three hydrogenated six-membered carbocyclic rings. The compd. of formulaIincludes those of formulas II and III. A pref. example of a compd. of the formula II is hydrogenated benzyltoluene and one of a compd. of the formula III is hydrogenated benzylbiphenyl.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a grease composition, and more particularly to a grease composition comprising a thickener and a synthetic naphthenic hydrocarbon oil.

Synthetic naphthenic hydrocarbons are used as base oils in grease compositions, but with the development of mechanical devices in which grease is used, it is necessary to select an appropriate grease to effectively function these mechanisms. Not only is it necessary, but it is also required to have high performance.

As the lubricant that serves as the base oil for ordinary grease compositions, a lubricating oil component manufactured from petroleum oil is used.

However, it is well known that such mineral oil-based oils, even if refined, do not have the performance to function satisfactorily under severe conditions. Therefore, it is common practice to add various additives to such lubricating oil components to improve the performance. However, even though the addition of additives may improve some types of performance, other problems such as increased corrosion and increased sludge formation arise, and adding additives is insufficient to improve performance. It is difficult to bring about.

As the recent driving conditions for mechanical equipment have become more severe,
It has become especially important to have a long lifespan.

The deterioration phenomenon is largely due to the oxidation of the lubricant f+l+ in the base oil, so the acid value of the base oil is stable t! 1 became an important issue for Koma. In addition, as the uses of grease have expanded, the number of products with a high 1-helix coefficient has also increased. , :.

Ministry of the Invention et al. 131 recognized that nanotene-based hydrocarbon oil is excellent as a base oil for grease compositions, has excellent acid value stability f1, and has excellent acid value stability f1, As a result of various studies on grease compositions that have excellent performance in applications, we have found that the base oil contains J-
It was recognized that the grease composition had excellent Ill performance and acid value stability, and the present invention was completed.

The present invention is based on the thickener J, and the general formula (wherein "1 is an alkyl group having 1 to 3 carbon atoms, R3, II' is an alkyl group, and R3, II' is a Each is an alkyl group having a carbon number of 1 to 3, and l, ox and n are 0
An integer of ~3, X is O or 1. A pour point of O''C or less consisting essentially of a naphthenic hydrocarbon having 19 to 30 carbon atoms and having at least three hydrogenated six-membered carbon rings of type b1 represented by

This is a grease composition consisting of a base oil having a traction coefficient of 0.08 or higher and a traction coefficient of 0.08 or higher. A known method b can be used. Examples of thickeners include lithium, barium, calcium, aluminum, soda, IJ/υ, and strontium. tsu()un<-,- Various metals
Combined J Luganoshi [l giraffes, clay, pen 1~nai 1~
．． ][]Idreid, graphite, etc.

The compounds represented by the general formula (2) include those represented by the following general formulas (I), J, and (II[).

R1 is an alkyl-substituted alkyne group having 1 to 3 carbon atoms or a linear nonol or 1-lene group, preferably a meblene group, ], dylene group, or a methyl-substituted medylene group (R1, R< Onibi 1 or 5 is an alkyl group having 1 to 3 carbon atoms, which may be the same or different (-), and preferably (,
1 meburu sin again [yoding del group.

21m, J, and η are integers from 0 to 3, preferably 0 to I, and =1. The number of carbon atoms in MaI Koai 81 is 19~
30, preferably [yo19~2/1. Better J, or 1
9 to -22.

Among the compounds not represented by the above general formula (II), hydrogenated dibenzyl 1-ru]nin, hydrogenated (benzylphenyl)phenylethane, or 1 to 2 methyl or ``pur WI conversions thereof are preferred; Among the compounds represented by the general formula (Ill), hydrogenated benzylbiphenyl or one or two methyl or ethyl substituted products thereof are suitable for the purpose of the present invention.

Examples of suitable compounds include hydrogenated dibenzyl-1-luene, hydrogenated 1.1-(benzylphenyl)phenylethane, hydrogenated 1.1-(benzyl-1-lyl)phenylethane, hydrogenated benzylbiphenyl, hydrogenated Examples include 1.1-(biphenylyl)7-nylni[tan], hydrogenated (ethylbiphenylyl)phenylmethane, hydrogenated 1.1-(ethylbiphenylyl)phenylethane, and hydrogenated methylbenzylphenyl.

These compounds, for example, hydrogenated dibenzyl toluene can be prepared by reacting hydrogenated benzyl with toluene in the presence of a free sol fluorocarbon catalyst W to form 1q dibenzyl 1.
- Obtained by hydrogenating toluene. J:/This hydrogenated benzyl biphenyl is obtained by hydrogenating benzyl biphenyl obtained by reacting benzyl monogenide and biphenyl in the presence of a Friedelta-Talanots catalyst. By doing so, it becomes 1;1.

The compound obtained in this way is a mixture of a single compound, and also a mixture with a partially hydride (according to the hydrogenation process A'1). However, separating only specific compounds from these mixtures is very tedious, and in many cases, it is difficult to separate only specific compounds from these mixtures. Therefore, it is not necessary to separate.As in A, in the sense of <7, the hydrogenation rate does not need to be completely 100%, but more than 80% or more than 90% in 1-11 minutes. be.

Further, the compound used in the present invention must have a pour point or crystal disappearance temperature of 0° C. or lower, an aniline point of 70° C. or higher, and a 1-Laxine coefficient of 0.08 or higher. Such compounds exhibit good performance when used as base oils in grease compositions.
The compounds used in the present invention have an acid value stability of a certain level or higher.
JIS K 2514
-1980 test method-) τ, viscosity ratio and total acid value increase (nag K Ol
-1/(J) and n-hebutane insoluble fraction (% effort)
are 1.2 or less, 0.3 or less, and J: and 0.31, respectively.
Preferably under a female.

The oxidation test was performed using 2,6-di[-butyl para-cresol and J
: A trial was conducted in which 0.5% by weight of each dialkyldidi-A zinc phosphate was added.

Oxidation test strip fI JT8 ΔS-T M K 2514-1980 D 2272-67 sample 300771,9 50Q damp
IG5,! i °C150℃ initial oxygen pressure
6.3kg/cm2 hours
72 hours - Oxidation catalyst Copper rice iron
Copper and iron The 1~Laxin coefficient here is b measured under the following conditions. 1 to luxion coefficient was measured using a So Iff cylindrical 1f friction tester. Traction (rolling friction) is achieved at three contact points between the central cylinder and three cylinders placed on the outside, and the same vertical cylinder φ acts on the contact points. . At this time, ■ is the average Hertzian pressure T O,! i75~
It is 1.157GPa. The other article 1'1 is a3 in Table 1.
It is.

Table 1 Traction experimental condition f! 1 Rotation speed 1.05~4.19771/S 3m
1lt O-+1.221n/S test Is cylinder Material Bearing steel 5UJ-2 Hardness 1-IV
760~800\J method Outer cylinder 40n+m
/ 9mm inner cylinder 40+nnm15TI1 moisturized Dripping method Flow rate Approximately 10 bar λ/min supply oil depletion The operating procedure for the 28℃ experiment is to first make the rotational speed constant for both the inner and outer cylinders, apply a weight, and then increase the rotational speed of the outer cylinder. By increasing the slip rate by -h 'it 1! L, η- Friction against slip ratio 1~
Changes in the torque or traffic coefficient were continuously determined. The friction 1 ~ torque is determined by measuring the torsional moment 1 ~ of the center free support 1 at the t1 tangent of the resistance wire strain.

The traction coefficient measured under this condition is
As the edge rate increases, it first stands straight,
After that, the maximum is set to 11/1 (I (showing a downward trend).

In this case, the <r region, which is particularly important from a practical standpoint, is light due to shearing of the oil film! 1 - This is the initial linear region where the heat is not large, and especially when the 1~ luxion coefficient of this region is less than ・j
Elephant and Zuru.

For example, the average Hertzian pressure is 1,157 Ql)a, the rotational speed is 4.19 m/S, and the J slip speed is 0,022 air/S.
1 to luxion coefficient measured at [j, Pufden-based ore 1IlI O,05 polyiso 1 brene hydride 0.06 1:1 to dicyclo 0,065 dicyclohexylethane 0.075 α-medylstyrene linear 0
．． Although it is a 09211 body hydride, the compound represented by the general formula (3) used in the present invention is 0.08 or more, and even exceeds 0.095.
It is extremely superior to these hydrocarbons.

The thickener, the compound represented by general formula I, and optional additives are mixed to form a grease composition.

Examples of additives include antioxidants, dispersants, viscosity index improvers, rust inhibitors, and anticorrosion agents.

The grease composition of the present invention can be used for ordinary grease applications, and can be particularly suitably used as a grease for rolling friction drive devices or a grease for rolling bearings. And the grease composition of the present invention,
While having the characteristics resulting from the fact that the base oil is a naphthenic hydrocarbon oil, it has the effect of having high oxidation stability and being able to be used for a long time in severe steel 1'1.

Next, the present invention will be explained in more detail with reference to Examples. In the following examples, "parts and 1" refer to small amounts unless otherwise specified.

Example 1 Aluminum chloride 0.002-0.0 in Torni I part
1 part was added and heated to 70°C, then 1 part of benzyl chloride was added and reacted for 2 hours. The reaction product was washed with water to remove the catalyst, and then distilled to separate unreacted substances. (The recovered dibenzyltoluene (mixture of m->p-〉〇-19-isomers) was supplied to O-1~Crepe, and using a nickel catalyst, an initial pressure of hydrogen was 40 kg/cm2G, and once at 200°C for 4 hours. Perform hydrogenation reaction to obtain dibenzyl hydrogen 1H■
(isomer mixture) was obtained.

To this hydrogenated naphthenic hydrocarbon oil, 0.5% by weight each of 2,6-ditertiary-butylvalacresol and zinc dialkyldithiophosphate were added as antioxidants.
An oxidation test was conducted under the conditions described above. Similar tests were conducted on compositions prepared from naphthenic hydrocarbon oils. Properties of hydrogenated naphthenic hydrocarbon oil (15) and test results are shown in Table 2 with other examples (71)
And as shown in Table 3, J0 is as shown in the table below. (JIS
According to K 2220-1980. )11-. A1: The additives used at this time were 0.5% by weight of antioxidant, 13% of extreme pressure additive type FF, and 1.5mm% of rust inhibitor.
Met.

Test item Test result Mixing G'J degree (2!i'C)
280 perfect score ('C) 18
5 Ash content (%) 0.9 Oxidation stability (ka/cm2) 0.3 (
99°Qx 100brs) Oil resistance a (%) 4.1 Mixing stability 1m 30G Kemzan type load capacity (Ib) 2.5 Leakage degree (130℃
x 6hrs) 3.2 Also in the following examples, grease compositions were made according to the performance of the base oil.

Example 2 Add 0.001 to 0.005'E of aluminum chloride to 4 moles of 1.1-Schiff J Niruthan, heat to 60'C, add 110% of 1 mole of benzyl chloride, and heat for 20 minutes.
2- Reacted. Next, the reaction product was washed with water to remove the catalyst, and then distilled to separate unreacted substances.

The obtained 1,1-(benzylphenyl)phenylethane (isomer mixture) was supplied to an autoclave and heated to an initial hydrogen pressure of 100 kQ and a temperature of 140 to 170°C using a nickel catalyst.
A hydrogenation reaction was carried out for 5 hours to obtain hydrogenated 1.1-(benzylphenyl)phenylethane (interisomer compound).

Example 3 Hydrogenation [noethyl-substituted 1.1-( benzylphenyl) (mixture with phenylethane) was obtained.

Example 4 7 methyl methane (1 sulfur) in the reactor
200 ml was supplied and kept at 15°C. Then a 1=1 mixture of methyldiphenylmethane and styrene 80
0? 71 (t) was added dropwise over 2 to 3 hours, during which time the temperature of the reaction solution was maintained at 15 to 20°C. After the dropwise addition, 200 ral of i!$1 sulfuric acid was added and the reaction was continued for 30 minutes. Repeatedly wash the reaction product with water [
) After removing sulfuric acid and distilling L.
-(Benzylphenyl)phenylethane was obtained. The mixture was then hydrogenated in the same manner as in Example 2 to obtain a mixture with hydrogenated monomethyl-substituted 1.1-(benzylphenyl)ethane).

Example 5 Aluminum chloride o, ooi ~ 0.0 to 5 parts of biphenyl
05 parts of benzyl chloride was added thereto, and the mixture was heated to 60° C., and then 1 part of benzyl chloride was added thereto and reacted for 20 minutes.

The reaction product was washed with water to remove the catalyst, and then distilled to separate unreacted substances. The obtained pendylbiphenyl (isomer mixture) was supplied to an autoclave at 1°C, and an initial hydrogen pressure of 100K (1/am2G, '
A hydrogenation reaction was carried out at an IQ degree of 140 to 170° C. for 2 hours to obtain hydrogenated benzyl biphenyl (isomer mixture).

Example 6 Hydrogenated pendyl monoediruvin was prepared by the same method as in Example 5, except that 5 parts of monoethylbiphenyl and 0.03 parts of aluminum chloride were used instead of biphenyl. Nil 15 - Example 7 To the reactor: 1-silbenpine 1°C Δj and 200.1 ml of concentrated sulfuric acid were fed and maintained at 15°C. Then, a 1:1 mixture of cyclohexylbenzene and styrene was added.
o, 4 was added dropwise over 2 to 3 hours, during which time the temperature of the reaction solution was maintained at 15 to 20°C.

After the dropwise addition was completed, 200 Tnl of a-sulfuric acid was added and the reaction was continued for 30 minutes. The reaction product was then repeatedly washed with water to remove sulfuric acid, and 1°1-(cyclohexylphenyl)phenylethane (a mixture of structural isomers) was obtained by distillation. Next, a to 1.1-<cyclohexylphenyl)phenylethane 1 was supplied to the A-tokrepe, and using a nickel catalyst, the hydrogen initial pressure was 100 kn/cm2G and the temperature was 140 to 170.
Hydrogenation was carried out at ℃ for 2 hours to obtain hydrogenation
Nilyl) phenylethane (mixture of structural isomers) was obtained.

16- Example 8 In Example 7, 800 ml of a 1:1 mixture of monoedil biphenyl and styrene was used instead of cyclohexylbenpine and the mixture of cyclohexylbenpine and styrene. Hydrogenation of 1.1-(ethylbiphenylyl)phenylethane by the same method except for Example 9 In Example 4, monomethylbenzyl chloride was used instead of biphenyl, the reaction temperature was 80°C, and the reaction time was 1 hour. Hydrogenated methylbenzylphenyl was produced in the same manner as in Example 4 except for this.

Procedure City i1 Motooth Showa L U7+ ', 12J] 21 E+ Commissioner of the Patent Office Name Kazuo Sugi Tono 1, Indication of matter A'1 1988 Special revision application No. 4,745 yen 2, Name of invention Grease composition Article 3, Ministerial affairs to be amended 1 Which relationship Patent applicant address 6-17-2 Ginza, Chuo-ku, Tokyo Name Title
(664) Shin [1 Honsei Kagaku Kogyo Co., Ltd. (and 1 other person) Representative Ministry Konan Daisou 4, Agent address: 5 Dia Palace Nibancho, 11-9 Nibancho, Chiyoff1-ku, Tokyo, Date of amendment order ``A'' Spontaneous correction 6, M-correct object 7, contents of correction Attachment ``A'', as shown in Book 4-, -Gajōgen υI□(.,,
11 Ming MI Ushi 1, Name of the Invention Grease Composition Claim 1 Thickener J, and General Formula L (wherein R1 is alkylene 3K having a carbon number of 1 to 3)
, R3, R' and 1)5 each independently have 1 carbon number
-3 Al 1-l group, and (1,1n and η
is an integer from O to 3, and x is O or 1. ) having a pour point of 0° C. or lower and consisting essentially of a naphthenic hydrocarbon having 19 to 30 carbon atoms and having at least one hydrogenated six-membered carbon ring.

A grease composition comprising a base oil having an aniline point of 70° C. or higher and a traction coefficient of 0.08 or higher.

The present invention relates to a grease composition, and more particularly, 1- refers to a grease composition comprising a thickener, a synthetic naphthenic hydrocarbon oil, and 9. a synthetic naphthenic hydrocarbon to a base oil of the grease composition. However, with the development of mechanical devices in which grease is used, 1. However, in order to effectively manage these structures, it is necessary to select an appropriate grease, and one that provides high performance is required.

The lubricating oil component produced from petroleum oil is used as the 1Ivl H'l agent, which is the base oil of ordinary grease compositions.

. However, even if this J: eel mineral oil-based product is refined, it is harsh (1-valve function IL in 7 conditions).
Therefore, it is common practice to add various additives to such lvI lubricating oils to improve their performance. However, adding additives can improve the f1 performance of a certain scale, but there are other problems such as an increase in M consumption and an increase in the amount of sludge produced (1 However, Kunisuke says that the addition of additives alone is sufficient to bring about the performance of the 4-gun.

As the operating conditions of modern mechanical equipment become more severe, longer lifespans are increasingly required. What is the deterioration phenomenon? Since the oxidation of the lubricating oil component is largely due to oxidation, the oxidation stability of the base oil has become a particularly important problem. In addition, as the uses of grease have expanded, the demand for greases with high coefficients of 1 to 3 has also increased.

The inventors of the present invention have recognized that naphthenic hydrocarbon oil has excellent performance as a base oil for grease compositions, has excellent oxidation stability, and has excellent f1 performance for rolling friction drive devices. Grease compositions containing a specific naphthenic hydrocarbon oil having three bonded and hydrogenated six-membered carbon rings as a base oil have been studied in various ways. It was recognized that the performance A'3 and oxidation stability were excellent, and the present invention was completed.

That is, the present invention provides thickeners and general formula I (wherein R1 is an alkylene group having 1 to 3 carbon atoms R
3, R4 and R'M; L- each independently has 1 to 1 carbon atoms;
3 is an alkyl group, and 2. bar and n are 0-3
is an integer, X is 0 or 1. 0°C consisting essentially of a naph7-based hydrocarbon having 19 to 30 carbon atoms and having three cycles of at least one hydrogenated six-membered carbon ring represented by
Pour point below.

A grease composition comprising a base oil having an aniline point of 70° C. or higher and a luxation coefficient of 0.08 or higher.

As the thickener used in the present invention, known thickeners can be used depending on the mode of use. Such thickeners and 1
In addition to various metal soaps such as lithium soap, barium soap, calcium soap, aluminum soap, soda soap, and strontium soap, we also use synthetic polymers, organojiro 1, clay, and bendable soap. , silica, graphite, etc. .

Compounds represented by the general formula (2) include those represented by the following general formula (If) Onibi (1#). .

R1 is Al-1 having 1 to 3 carbon atoms, VB-substituted Al-1;
- - or straight ff+ alene group, preferably tab1non JJ, :rf-lene group, methyl-substituted methylene group tealu R3* R' J-) J, HR5+,
tlm-mata is an alkyl group having 1 to 3 carbon atoms which may be different, and preferably I is a mebble group or an ethyl group.

ffi, 1rL and η are integers of O to 3, preferably 0 or 1, and the number of carbon atoms in compound 81 is 19 to 3.
30, preferably 19-24. More preferably 19~
It is 22.

Among the compounds represented by the above general formula (I), hydrogenated dibenzyltol, hydrogenated (benzylph[nyl)]
Preferred are nylcocne or 1-2 methyl or ethyl substituted products thereof, and among the compounds represented by the general formula ([), hydrogenated benzylbiphenyl or 1-2 methyl or ethyl substituted products thereof. Methyl or ethyl substitutions are preferred for the purposes of the present invention.

Examples of suitable compounds include hydrogenated dibenzyltoluene, hydrogenated 1.1-(benzylphenyl)phenylethane, hydrogenated 1.1-(benzyltolyl)phenylethane,
Hydrogenated benzylbiphenyl, hydrogenated 1.1-(biphenylyl)phenylethane, hydrogenated (-[tilbif J, nylyl)phenylmethane, hydrogenated 1.1-(ethylbiphenylyl)phenylethane, hydrogenated methylbenzylbiphenyl, etc. can be mentioned.

These compounds, for example, hydrogenated dibenzyltoluene, can be obtained by reacting a halogenated benzyl with toluene in the presence of a Friedelkraff catalyst and hydrogenating dibenzyltoluene. Further, hydrogenated benzyl dophenyl can be obtained by omitting hydrogenation of benzyl biphenyl obtained by reacting a halogenated benzyl and biphenyl in the presence of a Friedel-Craf catalyst.

The compounds obtained in this way are mixtures of isomers and, depending on the hydrogenation conditions, also mixtures with partially hydrogenated products. However, it is not only difficult to separate specific compounds from these mixtures;
In many cases, it is not necessary to separate I-I, as the intermediates also perform well for the purposes of the present invention. In this sense, the hydrogenation rate does not need to be completely 100%, but it is sufficient to make it 80% or more, preferably 90% or more.

In addition, the compound used in the present invention has a pour point or crystal disappearanceff1lf (refers to the temperature at which precipitated crystals completely dissolve by increasing the temperature) of 0°C or lower, and an aniline point of 70°C or higher. It is necessary to have a traction coefficient of .08 or more. Such compounds exhibit good performance when used as base oils in grease compositions. Furthermore, the compounds used in the present invention are more than a certain amount.
- It is necessary to have the oxidation stability of JTS
In the test method of K 2514-1980, an increase in viscosity ratio and total acid value (Ill!
IKO+-1/'g), J, and η-heptane insoluble content (Shigenobu %) are each 1.2 or less.

It is desirable that it be 0.3 or less and 0.3 or less e.

Further, it is desirable that the oxidation life (RBOT) defined in ΔSTM D2272-67 be 250 minutes or more, preferably 300 minutes or more. The oxidation test is carried out on samples to which 0.5 weight percent of each of 2,6-di-toptyl para-cresol and lead schiffurkyldithiophosphate is added.

Oxidation test conditions JIS ΔSTM K 2514-1980 [) 2272-67 test F4 m 3007711. 50g temperature 165.5℃ 150℃ initial lfl phosphorus pressure 6.3k (1/Cm2 intercostal
72 hours - Oxidation catalyst Copper and iron Copper and iron The traction coefficient herein is measured under the following conditions. The 1 helixcon coefficient was measured using a So ITI cylindrical If1wA tester. Traction (rolling red) is performed at three contact points between a central cylinder and three cylinders placed outside it, and the same vertical cylinder acts on the contact points. The blood pressure at the time is 0.57 as an average Hertzian pressure.
5-1, 157 GPa. Other conditions are as shown in Table 1.

Table 11-Raction experimental conditions Rotational speed 1.05 to 4,19 bar/S sliding speed
0~0.22m/S Test piece circle n Material Bearing steel S LJ J-2[1
i1' degree 1-1v 7 (liO~800 dimensions outer cylinder 40+nmX 9mm inner cylinder 40
mmX! imm (diameter x width) Lubrication method Dripping method Diversion Approx. 10m (1/min
Supply oil depletion 28℃ 8- In the experimental procedure, first, the rotational speed of the inner and outer cylinders was adjusted.
Keep it constant and load the weight! After ζ, the slippage rate was increased by increasing only the rotational speed of the outer cylinder, and changes in the friction torque or traction coefficient with respect to the slippage rate were continuously determined. Friction torque is measured by directly measuring the torsional moment of the central free support shaft using resistance line strain.

The traction coefficient measured under this regulation shows a tendency to first rise linearly as the revelry rate increases, and then to reach a maximum and then decline.

In this case, the area that is particularly important from a practical standpoint is the initial linear area where the heat generated by shearing the oil film is not large.
In particular, we will focus on the traction coefficient in this area below.

As an example, the traction coefficient measured at an average Hertzian pressure of 1.157 Gpa and a rotation speed of 4.19 mm/S and a shear speed of 0.022 mm/S is: Naphthenic mineral oil: 0.05 Polyisobutylene hydride: 0.06 mm cyclohexane
0.0659-°dicyclo to 4:silethane 0.075α-medylsdylene linear dimer hydride 0.09 However, the compound represented by the general formula 1 used in the present invention has a concentration of 0.08 or more, 0.095 It is extremely superior to these hydrocarbons.

A grease composition is prepared by mixing a thickener, a compound represented by the general formula (2), and additives added as necessary. Examples of additives include antioxidants, dispersants, viscosity index improvers, rust inhibitors, corrosion inhibitors, and the like.

The grease composition of the present invention can be used for ordinary grease applications, and can be particularly suitably used as a rolling SM drive device grease or a rolling bearing grease. The grease composition of the present invention has the characteristics resulting from the fact that its base oil is a naphthenic hydrocarbon oil, and also has the effect of having high oxidation stability ↑η and being able to be used for a long time under severe conditions.

Next, the present invention will be explained in more detail with reference to Examples. In addition, "part-1" in the following examples (-) is based on the amount of vehicles unless otherwise specified.

Example 1 1-Rue [23 parts to 0.002 parts aluminum chloride, 0
．． 01 part was added and heated to 70°C, then 1 part of benzyl chloride was added and reacted for 12 hours. 7j. The reaction product was washed with water to remove the catalyst, and then distilled to separate unreacted substances. jqed dibenzyl turquoise (m->p->O
-Unusual! 1 kg/cm2 G
The hydrogenation reaction was carried out at a temperature of 200°0 for 4 hours to yield 1 to 1 μl of dibenzyl hydride.

To this hydrogenated l,2'J hydrogenated hydrogen oil, 12,6-ditercydeleave bulvaracresol and 0.0% of oxidation inhibitor, 12,6-ditercydeleave bulvaracresol, and 0.00% of the 2'J hydrogen hydride oil were added. An oxidation test was carried out in accordance with the above-mentioned procedure with the addition of 5% by weight of Example 2. A1 test was conducted.The bamboo-like shape of hydrogenated nano-1 hydrocarbon oil and the test results were compared with other examples.
and shown in Table 3.

The hydrogenated dibenzyltoluene was mixed with j (oil (87%)) and 1
The properties of the grease composition thickened with lidium (13%) are as shown in the table below.
Based on SK 2220-1980. ). ',
J-dE, the additives used at this time were 0.5% by weight of antioxidant, 31% by weight of extreme pressure additive, and 1.5% by weight of rust inhibitor.

Test section [1 test result mixing Wa
lU (25℃) 28℃ point (℃)
185 Ash content (%) 0.9 Oxidation stability (kg/cn+2) 0.
3 (99℃ x 100brs) Oil content (%) 4.7 Mixing stability 306も\Ken type load capacity bamboo capacity (,91+) 2.5fli! i!
11 degrees (130℃ x (ihrs) 3.2
IZ- d3.1, about 1 during the execution of Suju (11 of B base Mt+
Grease compositions were made according to their functions.

11 rows of cusp 2 1.1-Dino[Nyl rtan/I'L-l to J oily aluminum, 0.001 to 0.00! Add ittle and heat to 60℃
1L of benzyl benzyl and reacted for 20 minutes.Then, the reacted material was washed with water.
) (After removing the catalyst), the mixture was distilled and the unreacted substances were separated.

11? The obtained 1, 1-(benzylphenyl)-nonyl 1-tane (Tatsumi↑Z1 body mixture) was supplied to 71-1-clay 1, and the initial pressure of C hydrogen was 100 k using a nickel catalyst.
g temperature 1'I O= 170°Cc5jIllll1 hydrogenation reaction t'lJ itintte hydrogenation 1.1 (benzyl-)I nyl) phenyl[tan (+R↑!1 mass mixture)
100 l.

Example 3 J) Same as Example 2, and instead of 1,1 sifte nil T tan, [)■Pull it#s1.1 -sheet r nil 1-tan 4■ru was used except for the example. 2. In the same manner, 1!N of hydrogenated EnotopurufitY operation 1,1 (mixture with benzylph[nyl)nyl-14-=13-] was added.

Example 4 In a reactor, methane was added at 1°C and concentrated sulfuric acid at 20°C.
0°C was supplied and maintained at 15°0. Next, 800 m of a 1:1 mixture of methane and styrene were added.
1 was added dropwise over a period of 2 to 3 hours, during which time the temperature of the reaction solution was maintained at 15 to 20°C. After completion of dropping, sulfuric acid 20
The reaction was continued for 30 minutes by adding 07rt (1k). Then, the reaction product was repeatedly washed with water + distilled with iX [remove acid 1) to obtain monomethyl-substituted 11.1-(benzylphenyl)phenylethane. Ta. Then, hydrogenation was performed in the same manner as in Example 2 to obtain hydrogenated monomethyl W-converted 1.1-(
A mixture of pendylphenyl)ethane CI-13 with CH3) was obtained.

Example 5 Aluminum chloride o, ooi~0.0 in 5 parts of Pino Jyl
05 parts was added, heated to 60°C, and then added C-bensilk [1
Add 5411 parts and react for 20 minutes.

The reaction product was washed with water to remove catalyst C, and then distilled to separate unreacted substances. The entire mixture of benzyl bif-J-nyl (!
/cm2 G, gilctl 10~170°Cte2
The hydrogenation reaction (j) yields hydrogenated benzylbiphenyl (isomer mixture) i1: .

Example 6 In Example 5, hydrogenated benzyl t noni [-f 1j mixture).

Example 7 Into the reactor, Schif[]1-Sylben L-1 and concentrated Ti
A temperature of 2007 nm was supplied and maintained at 15°C. Then, a 1:1 mixture of silbepine and subuurene, etc., was added dropwise to Schiff [1] over a period of 2 to 3 hours,
The temperature of the reaction solution was maintained at 15-20°C.

After dropping, add il:Q sulfuric acid 200?71,9 and continue the reaction for 30 minutes! /child. Then, the reaction product was repeatedly washed with water to remove C' IAM, and then subjected to distillation to give
[Nirni'thane 16- (isomer mixture) was obtained. Next, 1.1-(cyclo to 1"sylph]-nyl)fu'nilethane was fed at 1°C (!-Δ-talk no. 16-) to a nickel catalyst. Water cable first f using
, 'E 100 kg/cm 2 G,
The hydrogenation reaction was carried out at 2111 degrees Celsius (140-170 degrees Celsius) for 2 hours.
Nylethane (isomer mixture) 1! No Iko.

Example 8 In Example 7, d3, Schiff [] to = 1 silbenzene was replaced with 7-tylpino-nil 11 and cyclohexylbenzene was replaced with 7-t-delpino]nil in place of the mixture. 1:1 mixture with watermelon 800771.
Hydrogenation 1.1- in the same manner except that fl was used.
(1-bulbif, a mixture with [nilyl)-non-1-17-] is 1!1.

Example 9 The same method as in Example 4 was followed except that monomethylbenzyl chloride was used instead of pif-L-nil, the reaction temperature was 80°C, and the distance between reaction parts was changed by 1 ff. J: Produced dihydrogenated methylbenzylphenyl.

Continuation? 111 Official document January 28, 1981 Kazuo Wakasugi, Commissioner of the Patent Office1, Indication of the case, 1981 Patent Application No. 4.7/152, Name of invention Grease composition representative Imai Landlord5, Amendment order Daily spontaneous amendment 6, "Detailed explanation of the invention" column 7 for the specification subject to amendment, full text correction statement 11 submitted on December 21, 1980, for writing the details of the amendment
! Book I) In Table 2 on page 20, rl 61 J in the flash point row (Example 2 column) is corrected to N 60J.

1-

Claims (1)

[Claims] 1. Thickener and general formula I (wherein R+ is an alkylene group having 1 to 3 carbon atoms)
R3, R4 and J: and R5 each independently have 1 to 3 carbon atoms.
is an alkyl group, and λ, ML and n are O~3
is an integer, X is O or 1. ) A pour point of 0° C. or lower consisting essentially of a naphdenic hydrocarbon having 19 to 30 carbon atoms containing at least one hydrogenated six-membered six-membered ring represented by 3 f&]i. A grease composition comprising a base oil having an aniline point of 70°C or higher and a traction coefficient of 0.08 or higher.