KR100410724B1 - Grease composition for constant velocity joints - Google Patents

Grease composition for constant velocity joints Download PDF

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Publication number
KR100410724B1
KR100410724B1 KR1019970023290A KR19970023290A KR100410724B1 KR 100410724 B1 KR100410724 B1 KR 100410724B1 KR 1019970023290 A KR1019970023290 A KR 1019970023290A KR 19970023290 A KR19970023290 A KR 19970023290A KR 100410724 B1 KR100410724 B1 KR 100410724B1
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South Korea
Prior art keywords
constant velocity
calcium salt
grease composition
weight
calcium salts
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KR1019970023290A
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Korean (ko)
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KR980002219A (en
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꼬 하타케야마
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교도유시 가부시끼가이샤
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Publication of KR980002219A publication Critical patent/KR980002219A/en
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Abstract

본 발명은 등속조인트용 그리스 조성물에 관한 것으로서, 더욱 상세하게는 (a)기본유; (b)우레아 증감제; (c)몰리브덴 디설파이드; (d)산화왁스, 석유술폰산, 알킬아릴술폰산, 살리실산 및 페녹시화물의 칼슘염 또는 과염기의 칼슘염중에서 선택된 칼슘염 또는 과염기의 칼슘염; (e)금속을 함유하지 않은 황-인계 극압제; 그리고 (f)몰리브덴 디티오카바메이드가 필수적으로 함유되어 이루어져 있어, 우수한 내마모도와 박리억제효과를 나타내는 등속조인트용 그리스 조성물에 관한 것이다.The present invention relates to a grease composition for a constant velocity joint, and more particularly, to (a) a base oil; (b) urea sensitizers; (c) molybdenum disulfide; (d) calcium salts or overbased calcium salts selected from waxes, petrosulfonic acids, alkylarylsulfonic acids, calcium salts of salicylic acid and phenoxyhydrates or calcium salts of overbased; (e) sulfur-free extreme pressure agents without metal; And (f) molybdenum dithiocarbamaide is essentially contained, and relates to a grease composition for a constant velocity joint having excellent wear resistance and peeling inhibiting effect.

Description

등속조인트용 그리스(Grease) 조성물Grease composition for constant velocity joints

본 발명은 등속조인트용 그리스 조성물에 관한 것으로서, 더욱 상세하게는 볼(Ball)형의 고정식(Fixed) 및 유동식(Plunging) 등속조인트에 사용되는 그리스 조성물에 관한 것이다.The present invention relates to a grease composition for constant velocity joints, and more particularly, to a grease composition used for fixed and flown constant velocity joints of a ball type.

복잡한 롤링(Rolling)과 슬라이딩(Sliding) 운동이 진행되는 조인트 부분과 윤활처리가 된 등속 조인트(constant velocity joint)사이에는 매우 높은 접촉압력이 생긴다. 이는 비정상적인 마모와 금속피로를 일으키고 이어서 스폴링(Spalling), 즉 조인트 부분이 박리되는 현상을 야기시킨다. 본 발명에 대하여 좀더 자세하게 설명하면, 본 발명은 조인트의 마모를 효과적으로 줄이면서 또한 조인트 부분의 박리현상을 효과적으로 줄일 수 있는 윤활처리에 효과적인 등속조인트용 그리스 조성물에 관한 것이다.There is a very high contact pressure between the joint part where the complex rolling and sliding movements proceed and the lubricated constant velocity joint. This causes abnormal wear and metal fatigue, followed by spalling, i.e., peeling of the joint part. In more detail with respect to the present invention, the present invention relates to a grease composition for constant velocity joints effective in lubricating treatment that can effectively reduce the wear of the joint and also reduce the peeling of the joint portion.

등속조인트에 윤활제로 사용되는 종래의 그리스로는 리튬비누를 증감제로 하고 몰리브덴 디설파이드를 함유하고 있는 극압그리스, 그리고 리튬비누를 증감제로하고 황-인계 또는 납 나프탈레이트 같은 극압제와 몰리브덴 디설파이드를 함유하는 극압그리스 등이 있다. 그러나, 등속 조인트에 사용되는 상기의 그리스는 현재고성능의 자동차가 수행하는 극심한 운행조건을 항상 만족시키지는 못한다.Conventional greases used as lubricants for constant velocity joints include lithium soap as a sensitizer, extreme pressure grease containing molybdenum disulfide, lithium soap as a sensitizer, and extreme pressure agents such as sulfur-phosphorus or lead naphthalate and molybdenum disulfide. Extreme pressure grease. However, the above greases used for constant velocity joints do not always meet the extreme operating conditions of high performance automobiles.

최근에는 사륜구동(FF-Type)의 자동차대수가 빠른 속도로 증가하고 있고 이러한 자동차에 사용되는 등속 조인트는 가능한한 가볍고 작아야 한다. 유동식 조인트로 사용되는 더블 옵셋(Double offset)형과 X형 그루브(Cross Groove)형의 등속조인트 뿐만 아니라 고정식 조인트로 사용되는 버필드(Birfield) 조인트는 6개의 볼을 통하여 토오크가 전달되는 구조를 가지고 있다. 이러한 조인트는 높은 접촉압력하에서 회전하는 동안, 복잡한 롤링(Rolling)과 슬라이딩(Sliding)과 같은 복잡한 왕복운동을 일으키게 되고, 이에 볼과 볼이 접촉하는 금속 표면에 응력이 반복적으로 가해지므로 금속피로로 인하여 스폴링 현상이 이 부분에 일어나게 된다.In recent years, the number of four-wheel drive (FF-Type) vehicles has been increasing rapidly, and the constant velocity joints used in such automobiles should be as light and small as possible. As well as the double offset and X Groove type constant velocity joints used as the floating joints, the Burfield joints used as the fixed joints have a structure in which torque is transmitted through six balls. have. These joints cause complex reciprocating motions such as complex rolling and sliding during rotation under high contact pressure, and due to the metal fatigue, the stress is repeatedly applied to the metal surface where the ball is in contact with the ball. The spalling phenomenon occurs in this area.

최근에는 엔진의 동력을 향상시키기 위하여 종래의 엔진과 비교할때, 접촉압력을 증가시키는데 많은 노력을 기울이고 있다. 이러한 예로서 연료 소비효율을 향상시키기 위하여 자동차의 경우는 경량화되는 추세이고, 조인트의 크기도 역시 작아지고 있다. 이러한 현상은 상대적으로 접촉압력을 상대적으로 증가시키게 되는바, 종래의 그리스로는 충분히 박리현상을 줄일 수 없어서 효과적이지 못하다. 또한, 그리스는 열저항성이 향상되어야만 하였다.Recently, much effort has been made to increase the contact pressure when compared with a conventional engine to improve the power of the engine. As an example, in order to improve fuel consumption efficiency, automobiles are lighter in weight, and joint sizes are also smaller. This phenomenon relatively increases the contact pressure, the conventional grease is not effective enough can not reduce the peeling phenomenon. In addition, grease had to be improved in heat resistance.

따라서 본 발명은 우수한 박리억제 효과와 열저항성을 가지면서 등속조인트에 적합한 새로운 그리스 조성물을 제공하는데 그 목적이 있다.Accordingly, an object of the present invention is to provide a new grease composition suitable for a constant velocity joint while having an excellent peeling inhibiting effect and heat resistance.

본 발명의 발명자들은 등속조인트의 부분적인 마모를 최소화하고 비정상적인 마모와 금속피로로 인한 금속의 박리현상을 없애고 열저항성을 가질 수 있는 그리스 조성물을 개발하기 위하여 많은 노력을 하였다. 본 발명자들은 복잡한 롤링(Rolling)과 슬라이딩(Sliding)과 같은 복잡한 왕복운동이 수행되는 윤활조건하에서 사용된 그리스의 성능평가를 하였다. 이때, SRV(Schwingungs Reibung und Verschleiss) 시험기로 호칭되고 있는 진동마찰마모 시험기를 사용하여 여러 종류의 증감제, 고체 윤활제 또는 첨가제를 배합하여 마찰계수와 마모성과 같은 윤활성질을 측정하였다.The inventors of the present invention have made a lot of efforts to minimize the partial wear of the constant velocity joint, to eliminate the delamination of the metal due to abnormal wear and metal fatigue, and to develop a grease composition that can have heat resistance. The inventors have evaluated the performance of greases used under lubricating conditions in which complex reciprocating motions such as complex rolling and sliding are performed. At this time, various types of sensitizers, solid lubricants or additives were mixed using a vibration friction tester, which is called a Schwingungs Reibung und Verschleiss (SRV) tester.

그 결과 기본유, 우레아 증감제, 몰리브덴 디설파이드, 특정 화합물의 칼슘 염 또는 과염기의 칼슘염, 금속이 함유되지 않은 황-인계 극압제, 그리고 몰리브덴 디티오카바메이트을 특정비율로 배합하여 이루어진 본 발명의 그리스는 우수한 마찰계수, 저마모도 같은 원하는 윤활성질이 나타나고, 또한 실제로 등속조인트를 사용하여 내구성 시험을 해본 결과, 등속조인트에 쓰이던 종래의 그리스와는 달리 본 발명의 그리스는 어떠한 박리현상도 일어나지 않음을 확인함으로써 본 발명을 완성하였다.As a result, the base oil, the urea sensitizer, the molybdenum disulfide, the calcium salt or the overbased calcium salt of a specific compound, the sulfur-phosphorus extreme pressure-free metal-free, and the molybdenum dithiocarbamate The grease exhibits the desired lubricating properties such as excellent coefficient of friction and low wear, and in fact, the endurance test using the constant velocity joint shows that unlike the conventional grease used for the constant velocity joint, the grease of the present invention does not cause any peeling phenomenon. The present invention was completed by confirming.

본 발명은The present invention

(a)기본유;(a) basic oils;

(b)우레아 증감제;(b) urea sensitizers;

(c)몰리브덴 디설파이드;(c) molybdenum disulfide;

(d)산화왁스의 칼슘염, 석유술폰산의 칼슘염, 알킬아릴술폰산의 칼슘염, 살리실산의 칼슘염, 페녹시화물의 칼슘염, 산화왁스의 과염기칼슘염, 석유술폰산의과염기칼슘염, 알킬아릴술폰산의 과염기칼슘염, 살리실산의 과염기칼슘염 및 페녹시화물의 과염기칼슘염 중에서 선택된 칼슘염 또는 과염기의 칼슘염;(d) Calcium salts of wax, calcium salts of petroleum sulfonic acid, calcium salts of alkylarylsulfonic acid, calcium salts of salicylic acid, calcium salts of phenoxylates, overbased calcium salts of wax oxides, overbased calcium salts of petrosulfonic acid, alkyl Calcium salts or overbased calcium salts selected from overbased calcium salts of arylsulfonic acid, overbased calcium salts of salicylic acid, and overbased calcium salts of phenoxylates;

(e)금속을 함유하지 않은 황-인계 극압제; 그리고(e) sulfur-free extreme pressure agents without metal; And

(f)몰리브덴 디티오카바메이드가 필수적으로 함유된 등속조인트용 그리스 조성물을 그 특징으로 한다.(f) It is characterized by the grease composition for constant velocity joints which essentially contains molybdenum dithiocarbamade.

이와같은 본 발명을 더욱 상세히 설명하면 다음과 같다.Referring to the present invention in more detail as follows.

본 발명의 등속조인트용 그리스 조성물은 성분(a)로서 기본유을 사용하는 바, 그 종류로는 광물유, 에스테르계 합성유, 에테르계 합성유, 탄화수소계 합성유 및 이들의 혼합물 중에서 선택된 윤활유를 사용함이 바람직하지만 본 발명이 이에 의해 한정되는 것은 아니다.The grease composition for the constant velocity joint of the present invention uses a base oil as component (a), and the kind thereof is preferably a lubricant selected from mineral oil, ester synthetic oil, ether synthetic oil, hydrocarbon synthetic oil and mixtures thereof. The invention is not limited by this.

성분(b)로서 우레아 증감제를 사용하는 바, 그 종류로는 디우레아 화합물 또는 폴리우레아 화합물이 바람직하지만 본 발명이 이에 한정되는 것은 아니다.When the urea sensitizer is used as component (b), the diurea compound or the polyurea compound is preferable as the kind, but the present invention is not limited thereto.

예를 들면, 디우레아 화합물은 모노아민과 디이소시아네이트를 반응시켜 얻어진 화합물이다. 디이소시아네이트의 예로는 페닐렌 디이소시아네이트, 디페닐 디이소시아네이트, 페닐 디이소시아네이트, 디페닐메탄 디이소시아네이트, 옥타데칸 디이소시아네이트, 데칸 디이소시아네이트 그리고 헥산 디이소시아네이트를 포함한다. 모노아민으로는 옥틸아민, 도데실아민, 헥사데실아민, 옥타데실아민, 올레일아민, 아닐린, p-톨루이딘 그리고 시클로헥실아민을 포함한다.For example, a diurea compound is a compound obtained by making monoamine and diisocyanate react. Examples of diisocyanates include phenylene diisocyanate, diphenyl diisocyanate, phenyl diisocyanate, diphenylmethane diisocyanate, octadecane diisocyanate, decane diisocyanate and hexane diisocyanate. Monoamines include octylamine, dodecylamine, hexadecylamine, octadecylamine, oleylamine, aniline, p-toluidine and cyclohexylamine.

또한, 폴리우레아 화합물의 예로는 디아민과 디이소시아네이트를 반응하여 얻어진 화합물이다. 디이소시아네이트의 예로는 상기한 바와 같고, 디아민으로는에틸렌디아민, 프로판디아민, 부탄디아민, 헥산디아민, 옥탄디아민, 페닐렌디아민, 톨루엔디아민 그리고 크실렌디아민을 포함한다.In addition, examples of the polyurea compound are compounds obtained by reacting diamine and diisocyanate. Examples of diisocyanates are as described above, and diamines include ethylenediamine, propanediamine, butanediamine, hexanediamine, octanediamine, phenylenediamine, toluenediamine and xylenediamine.

우레아 증감제로서 더욱 바람직하기로는 아닐린, p-톨루이딘, 시클로헥실아민 또는 이들의 혼합물과 같은 아릴아민을 디이소시아네이트와 반응시켜 제조한 것이다. 디우레아 화합물에서 아릴기는 탄소원자수 6 ∼ 7이고, 디우레아 화합물 내에서 아릴기의 비는 아릴기와 시클로헥실기의 전체 몰수를 기준으로 할 때, 0 ∼ 100 몰%가 바람직하다.More preferably as urea sensitizers are those prepared by reacting arylamines such as aniline, p-toluidine, cyclohexylamine or mixtures thereof with diisocyanates. In the diurea compound, the aryl group has 6 to 7 carbon atoms, and the ratio of the aryl group in the diurea compound is preferably 0 to 100 mol% based on the total moles of the aryl group and the cyclohexyl group.

성분(c)로서 몰리브덴 디설파이드를 사용하는 바, 이는 극압제로서 널리 사용된다. 윤활 메카니즘을 고려하면, 몰리브덴 디설파이드는 충격자구조를 가지고 있어서 얇은 층을 형성하면서 슬라이딩 운동에 의하여 쉽게 절단된다. 이로써 조인트의 시저(Seizure)효과를 방지하며, 마찰력을 감소하는 효과를 보인다.Molybdenum disulfide is used as component (c), which is widely used as an extreme pressure agent. Considering the lubrication mechanism, molybdenum disulfide has an impactor structure and is easily cut by sliding motion while forming a thin layer. This prevents the Seizure effect of the joint and reduces the frictional force.

상기 몰리브덴 디설파이드는 다양한 입자 크기로 제조될 수 있으며, 본 발명에서는 피셔법(Fisher Sub-Sieve sizer를 사용함)에 의하여 측정된 평균입자크기가 0.25 ∼ 10㎛ 범위의 것을 사용하며, 더욱 바람직하기로는 0.55 ∼ 0.85㎛ 범위의 것을 사용한다.The molybdenum disulfide may be prepared in a variety of particle sizes, in the present invention, the average particle size measured by the Fischer method (using Fisher Sub-Sieve sizer) is used in the range of 0.25 ~ 10㎛, more preferably 0.55 Use in the range of -0.85 탆.

성분(d)로서 사용될 수 있는 칼슘염 또는 과염기의 칼슘염으로는 엔진오일과 같은 윤활유, 산화왁스의 칼슘염, 윤활유 성분중의 방향족 탄화수소를 술폰화하여 얻은 석유술폰산의 칼슘염, 합성술폰산의 칼슘염(예를들면 디노닐나프탈렌술폰산 및 알킬벤젠술폰산, 알킬벤젠술폰산), 살리실산의 칼슘염, 페녹시화물의 칼슘염, 산화왁스의 과염기칼슘염, 석유술폰산의 과염기칼슘염, 알킬아릴술폰산의 과염기칼슘염, 살리실산의 과염기칼슘염 및 페녹시화물의 과염기칼슘염 등에서 선택하여 사용한다. 상기 나열된 칼슘염들은 금속세정 분산제 또는 녹방지제(rust inhibitor)로 잘 알려져 있다.Calcium salts or overbased calcium salts that can be used as component (d) include lubricating oils such as engine oil, calcium oxide of wax oxide, calcium salts of petroleum sulfonic acid obtained by sulfonating aromatic hydrocarbons in lubricating oil components, and synthetic sulfonic acid. Calcium salts (e.g. dinonylnaphthalenesulfonic acid and alkylbenzenesulfonic acid, alkylbenzenesulfonic acid), calcium salts of salicylic acid, calcium salts of phenoxylates, overbased calcium salts of wax oxides, overbased calcium salts of petrosulfonic acid, alkylaryls It is selected from overbased calcium salt of sulfonic acid, overbased calcium salt of salicylic acid, and overbased calcium salt of phenoxychloride. The calcium salts listed above are well known as metal cleaning dispersants or rust inhibitors.

성분(e)로서 금속이 함유되지 않는 황-인계 극압제를 사용하는 바, 이는 15 ~ 35 중량%의 황(S)성분과 0.5 ∼ 3 중량%의 인(P)성분으로 이루어져 있고, 황과 인의 성분 함량비를 적절히 조절하면 내마모효과(wear-resistant effect) 및 시저 억제효과(seizure- inhibitory effect)을 얻을 수 있다. 만약 황 성분의 함량이 상기의 범위를 초과하면 조인트가 쉽게 부식될 수 있고, 인 성분의 함량이 상기의 범위를 초과하면 마모억제효과를 얻을 수 없다. 또한 이들이 상기의 범위 미만으로 함유되면 본 발명에서 요구하는 효과를 얻을 수 없다.As the component (e), a sulfur-free extreme pressure agent containing no metal is used, which is composed of 15 to 35% by weight of sulfur (S) and 0.5 to 3% by weight of phosphorus (P). Properly adjusting the phosphorus content ratio can provide a wear-resistant effect and a seizure-inhibitor effect. If the sulfur content exceeds the above range, the joint can be easily corroded, and if the content of phosphorus exceeds the above range, the wear inhibiting effect cannot be obtained. Moreover, when they contain less than the said range, the effect calculated | required by this invention cannot be acquired.

성분(f)로서 몰리브덴 디티오카바메이트를 사용하는 바, 그 화학식은 다음과 같다.When molybdenum dithiocarbamate is used as component (f), the chemical formula is as follows.

[화학식 1][Formula 1]

Figure pat00001
Figure pat00001

상기 화학식 1에서, R1및 R2은 각각 탄소원자수 1 ∼ 24의 알킬기, 바람직하기로는 3 ∼ 18의 알킬기이고; m은 0 ∼ 3이고, n은 4 ~ 1이며, 단 m + n = 4이다.In Formula 1, R 1 and R 2 are each an alkyl group having 1 to 24 carbon atoms, preferably an alkyl group having 3 to 18 carbon atoms; m is 0-3, n is 4-1, and m + n = 4.

또한, 본 발명의 그리스 조성물은 필요에 따라 산화방지제, 부식방지제 및 녹방지제 중에서 선택된 하나 또는 그 이상의 것을 상기 필수성분에 첨가하여 사용할 수도 있다.In addition, the grease composition of the present invention may be used by adding one or more selected from antioxidants, corrosion inhibitors and rust inhibitors to the essential components as necessary.

본 발명의 등속조인트용 그리스 조성물은 조성물의 총량에 대하여 성분(a)의 기본유가 52.0 ~ 97.8 중량%, 성분(b)의 우레아 증감제가 1 ∼ 25 중량%, 성분(c)의 몰리브덴 디설파이드가 0.5 ~ 5.0 중량%, 성분(d)의 칼슘염 또는 과염기의 칼슘염이 0.5 ∼ 15 중량%, 성분(e)의 금속이 함유되지 않은 황-인계 극압제가 0.1 ∼ 3 중량%, 그리고 성분(f)의 몰리브덴 디티오카바메이트 0.1 ∼ 5 중량%가 함유되어 있다.The grease composition for constant velocity joint of the present invention has a base oil of component (a) of 52.0 to 97.8% by weight, 1 to 25% by weight of urea sensitizer of component (b) and molybdenum disulfide of component (c) based on the total amount of the composition. To 5.0% by weight, 0.5 to 15% by weight of calcium salt of component (d) or calcium salt of overbased, 0.1 to 3% by weight of sulfur-phosphoric extreme pressure agent which does not contain metal of component (e), and 0.1-5 weight% of molybdenum dithiocarbamate of f) is contained.

상기 그리스 조성물에 있어서 성분(b)의 함량이 1 중량% 미만이면 증감제로서 작용할 수 없고 본 발명에서 목적으로 하는 그리스 조성물은 얻을 수 없으며, 25 중량%를 초과하면 너무 딱딱해서 그리스 조성물에 요구되는 효과를 얻을 수 없다.If the content of component (b) in the grease composition is less than 1% by weight, it cannot function as a sensitizer and the grease composition intended in the present invention cannot be obtained, and if it exceeds 25% by weight, it is too hard to be required for the grease composition. No effect is obtained.

성분(c)의 함량이 0.5 중량% 미만, 성분(d)의 함량이 0.5 중량% 미만, 성분(e)의 함량이 0.1 중량%미만 그리고 성분(f)의 함량이 0.1 중량% 미만이면 본 발명의 그리스 조성물에 요구되는 효과를 나타낼 수 없다. 또한, 성분(c)의 함량이 5 중량%를 초과, 성분(d)의 함량이 15 중량%를 초과, 성분(e)의 함량이 3 중량%를 초과, 그리고 성분(f)의 함량이 5 중량%를 초과하면 더 이상의 개선된 효과를 기대할 수 없고, 이 성분들은 오히려 본 발명의 박리억제 효과에 반대영향을 끼친다.The present invention is less than 0.5% by weight of component (c), less than 0.5% by weight of component (d), less than 0.1% by weight of component (e) and less than 0.1% by weight of component (f). The effect required for the grease composition cannot be exhibited. In addition, the content of component (c) is more than 5% by weight, the content of component (d) is more than 15% by weight, the content of component (e) is more than 3% by weight, and the content of component (f) is 5 If the weight percentage is exceeded, no further improved effect can be expected, and these components rather have an opposite effect on the peeling inhibiting effect of the present invention.

상기와 같은 본 발명을 다음의 실시예와 비교예에 의해 더욱 상세히 설명하면 다음과 같은바, 본 발명이 이에 한정되는 것은 아니다.If the present invention as described above in more detail by the following examples and comparative examples as follows, the present invention is not limited thereto.

실시예 1 ∼ 9 및 비교예 1 ~ 3Examples 1-9 and Comparative Examples 1-3

기본유 4100g과 디페닐메틸메탄-4,4'-디이소시아네이트 1012g을 컨테이너에 넣고 혼합한 다음, 70 ~ 80 ℃까지 가열하였다. 또 다른 컨테이너에는 기본유 4100g, 시클로헥실아민 563g 그리고 아닐린 225g을 첨가하여 70 ∼ 80℃까지 가열하였다. 이 혼합물을 충분히 교반시키면서 30분동안 반응시키고, 계속 교반하면서 반응계의 온도를 160℃ 상승시킨 다음, 온도를 냉각하여 베이스 우레아 그리스(base urea grease)를 제조하였다.4100 g of base oil and 1012 g of diphenylmethylmethane-4,4'-diisocyanate were placed in a container, mixed, and heated to 70 to 80 ° C. In another container, 4100 g of base oil, 563 g of cyclohexylamine, and 225 g of aniline were added and heated to 70 to 80 ° C. The mixture was reacted for 30 minutes with sufficient stirring, the temperature of the reaction system was raised to 160 ° C. while the stirring was continued, and the temperature was cooled to prepare a base urea grease.

다음 표 1에 제시된 배합비율로 첨가제를 상기의 베이스 그리스에 첨가하고, 임의로 기본유를 첨가한 다음, 쓰리-스테이지 롤 밀(three-stage roll mill)에서 혼합하여 혼합물의 침투도(penetration)가 No. 1 등급인 그리스 조성물을 제조하였다.The additive is added to the base grease at the mixing ratio shown in the following Table 1, optionally base oil is added, and then mixed in a three-stage roll mill to have a penetration ratio of No. . A grade 1 grease composition was prepared.

실시예 10Example 10

기본유 440g과 디페닐메틸메탄-4,4'-디이소시아네이트 58.9g을 컨테이너에 넣고 혼합한 다음, 70 ~ 80℃까지 가열하였다. 또 다른 컨테이너에는, 기본유 440g, 옥틸아민 61.1g을 첨가하여 70 ∼ 80℃까지 가열하였다. 이 혼합물을 충분히 교반시키면서 30분동안 반응시키고, 계속 교반하면서 반응계의 온도를 160℃상승시킨 다음, 온도를 냉각하여 베이스 지방족아민 우레아 그리스(base aliphatic amine urea grease)를 제조하였다.440 g of base oil and 58.9 g of diphenylmethylmethane-4,4'-diisocyanate were added to a container, mixed, and then heated to 70 to 80 ° C. To another container, 440 g of base oil and 61.1 g of octylamine were added and heated to 70 to 80 ° C. The mixture was allowed to react for 30 minutes with sufficient stirring, and the temperature of the reaction system was increased to 160 ° C. while the stirring was continued. Then, the temperature was cooled to prepare a base aliphatic amine urea grease.

다음 표 1에 제시된 배합비율로 첨가제를 상기의 베이스 그리스에 첨가하고, 임의로 기본유를 첨가한 다음, 쓰리-스테이지 롤 밀(three-stage roll mill)에서 혼합하여 혼합물의 침투도(penetration)가 No. 1 등급인 그리스 조성물을 제조하였다.The additive is added to the base grease at the mixing ratio shown in the following Table 1, optionally base oil is added, and then mixed in a three-stage roll mill to have a penetration ratio of No. . A grade 1 grease composition was prepared.

상기 실시예와 비교예의 그리스 조성물 제조시 사용된 기본유는 다음과 같은 조성을 갖는다.The base oil used in the preparation of the grease compositions of Examples and Comparative Examples has the following composition.

기본유의 종류: 광물유(mineral oil)Type of basic oil: mineral oil

점도(Viscosity): 157 ㎟/s (40℃에서)Viscosity: 157 mm2 / s (at 40 ° C)

14 ㎟/s (100℃에서)14 mm2 / s (at 100 ℃)

점도지순(Viscosity Index): 88Viscosity Index: 88

또한, 비교예 4는 몰리브덴 디설페이트, 황-인계 극압제 및 납 나프탈레이트를 함유하고 있으며, 시중에서 시판되는 리튬그리스이다.Comparative Example 4 also contains molybdenum disulfate, a sulfur-phosphorus extreme pressure agent and lead naphthalate, and is commercially available lithium grease.

[실험예]Experimental Example

다음의 측정방법에 의해 그리스의 물리적 성질을 측정하였고, 그 결과는 다음 표 1에 나타내었다.The physical properties of the grease were measured by the following measurement method, and the results are shown in Table 1 below.

침투도(penetration)Penetration

ISO 2137에 제시된 방법에 의해 측정하였다.It was measured by the method given in ISO 2137.

초적점(Dripping Point)Dripping Point

ISO 2176에 제시된 방법에 의해 측정하였다.It was measured by the method given in ISO 2176.

SRV 시험SRV test

시험편: - 볼(ball): 직경 10 mm (SUJ-2)Test piece: Ball: 10 mm diameter (SUJ-2)

- 원통형판: 직경 24 mm×7.85 mm (SUJ-2)Cylindrical plate: 24 mm diameter x 7.85 mm (SUJ-2)

측정조건:Measuring conditions:

- 하중: 500NLoad: 500 N

- 주파수: 15HzFrequency: 15 Hz

- 진폭: 3000㎛Amplitude: 3000㎛

- 시간: 10분-Time: 10 minutes

- 측정온도: 25℃-Measuring temperature: 25 ℃

- 측정항목; 최대 마찰계수, 볼에서 관찰되는 마모자국의 평균 지름(mm),-Metrics; Maximum coefficient of friction, average diameter of wear marks observed in the ball (mm),

표면에서 관찰되는 마모의 최대 깊이(㎛)Maximum depth of wear observed on the surface (μm)

실제 조인트를 사용한 작업대 상에서의 내구성시험Durability test on work bench using real joint

실제 조인트를 사용하여 작업대 상에서의 내구성 시험을 다음과 같은 조건으로하여 실시하여 박리정도를 측정하였다.The degree of peeling was measured by carrying out the durability test on the work bench using the actual joint under the following conditions.

측정조건:Measuring conditions:

- 회전수: 1000 rpmRPM: 1000 rpm

- 토크(torque): 392 NㆍmTorque: 392 Nm

- 조인트 각도: 8°Joint angle: 8 °

- 측정시간: 100 시간 운전 후-Measurement time: 100 hours after driving

- 사용된 조인트 형태: 버필드 조인트(Birfield Joint)Joint type used: Burfield Joint

X형 그루브 조인트(Cross Groove Joint)Cross Groove Joint

측정항목: 운전 후 각 부분의 박리현상의 유무Measurement item: Exfoliation phenomenon of each part after operation

[표 1]TABLE 1

Figure pat00004
Figure pat00004

Figure pat00005
Figure pat00005

상술한 바와 같이, 본 발명의 등속조인트용 그리스 조성물은 (a)기본유; (b)우레아 증감제; (c)몰리브덴 디설파이드; (d)특정의 칼슘염 또는 특정의 과염기의 칼슘염; (e)금속을 함유하지 않는 황-인계 극압제; (f)몰리브덴 디티오카바메이트 성분을 필수적으로 함유하고 있고, 이 조성물을 상기 실시예와 비교예의 시험의 결과비교로부터 명백히 알 수 있듯이 우수한 내마모 효과와 우수한 박리억제 효과가 있다.As described above, the grease composition for constant velocity joints of the present invention comprises (a) a base oil; (b) urea sensitizers; (c) molybdenum disulfide; (d) specific calcium salts or calcium salts of certain overbased; (e) sulfur-free extreme pressure agents containing no metal; (f) A molybdenum dithiocarbamate component is essentially contained, and this composition has an excellent wear resistance effect and an excellent peeling inhibiting effect, as can be clearly seen from the comparison of the results of the tests of the examples and the comparative examples.

Claims (4)

(a) 기본유 52.0∼97.8 중량% ;(a) 52.0 to 99.8 wt% of base oil; (b) 우레아 증감제 1∼25 중량% ;(b) 1 to 25% by weight of a urea sensitizer; (c) 몰비브덴 디설파이드 0.5∼5.0 중량% ;(c) 0.5 to 5.0% by weight of molybdenum disulfide; (d) 산화왁스의 칼슘염, 석유술폰산의 칼슘염, 알킬아릴술폰산의 칼슘염, 살리실산의 칼슘염, 페녹시화물의 칼슘염, 산화왁스의 과염기칼슘염, 석유술폰산의 과염기칼슘염, 알킬아릴술폰산의 과염기칼슘염, 살리실산의 과염기칼슘염 및 페녹시화물의 과염기칼슘염 중에서 선택된 칼슘염 또는 과염기의 칼슘염 0.5∼15 중량% ;(d) calcium salt of wax oxide, calcium salt of petrosulfonic acid, calcium salt of alkylarylsulfonic acid, calcium salt of salicylic acid, calcium salt of phenoxyhydrate, overbased calcium salt of wax oxide, overbased calcium salt of petrosulfonic acid, 0.5-15% by weight of calcium salt or overbased calcium salt selected from overbased calcium salt of alkylarylsulfonic acid, overbased calcium salt of salicylic acid and overbased calcium salt of phenoxylate; (e) 금속을 함유하지 않은 황-인계 극압제 0.1∼3 중량% ; 그리고(e) 0.1 to 3% by weight of a sulfur-phosphorus extreme pressure agent containing no metal; And (f) 몰리브덴 디티오카바메이트 0.1∼5중량%가(f) 0.1 to 5% by weight of molybdenum dithiocarbamate 필수적으로 함유되어 이루어진 것을 특징으로 하는 등속조인트용 그리스 조성물.Grease composition for a constant velocity joint, characterized in that consisting essentially. 제 1 항에 있어서, 상기 금속이 함유되지 않은 황-인계 극압제는 황(sulfur) 성분 15∼35 중량%와 인(phosphorus)성분 0.5∼3 중량%를 함유하고 있는 것을 특징으로 하는 등속조인트용 그리스 조성물.2. The constant velocity joint of claim 1, wherein the sulfur-free extreme pressure agent containing no metal contains 15 to 35 wt% of a sulfur component and 0.5 to 3 wt% of a phosphorus component. Grease composition. 제 1 항에 있어서, 상기 등속조인트는 등속 유동식 볼형 조인트 (constantvelocity plunging ball joint)인 것을 특징으로 하는 등속조인트용 그리스 조성물.The grease composition for a constant velocity joint according to claim 1, wherein the constant velocity joint is a constantvelocity plunging ball joint. 제 1 항에 있어서, 상기 등속조인트는 등속 고정식 볼형 조인트(constant velocity fixed ball joint)인 것을 특징으로 하는 등속조인트용 그리스 조성물.The grease composition for a constant velocity joint according to claim 1, wherein the constant velocity joint is a constant velocity fixed ball joint.
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JP4864296B2 (en) 2004-07-01 2012-02-01 協同油脂株式会社 Grease composition for constant velocity joint and constant velocity joint enclosing it
JP2006096949A (en) * 2004-09-30 2006-04-13 Toyoda Mach Works Ltd Grease composition for ball type constant velocity joint and ball type constant velocity joint
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JP5132170B2 (en) * 2007-03-22 2013-01-30 日本精工株式会社 Diurea grease composition
JP5399203B2 (en) * 2009-10-22 2014-01-29 Ｎｔｎ株式会社 Fixed type constant velocity universal joint
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