KR100562129B1 - Grease composition for constant velocity joints - Google Patents
Grease composition for constant velocity joints Download PDFInfo
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- KR100562129B1 KR100562129B1 KR1020040099944A KR20040099944A KR100562129B1 KR 100562129 B1 KR100562129 B1 KR 100562129B1 KR 1020040099944 A KR1020040099944 A KR 1020040099944A KR 20040099944 A KR20040099944 A KR 20040099944A KR 100562129 B1 KR100562129 B1 KR 100562129B1
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M101/00—Lubricating compositions characterised by the base-material being a mineral or fatty oil
- C10M101/02—Petroleum fractions
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M115/00—Lubricating compositions characterised by the thickener being a non-macromolecular organic compound other than a carboxylic acid or salt thereof
- C10M115/08—Lubricating compositions characterised by the thickener being a non-macromolecular organic compound other than a carboxylic acid or salt thereof containing nitrogen
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M127/00—Lubricating compositions characterised by the additive being a non- macromolecular hydrocarbon
- C10M127/02—Lubricating compositions characterised by the additive being a non- macromolecular hydrocarbon well-defined aliphatic
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M137/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing phosphorus
- C10M137/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing phosphorus having no phosphorus-to-carbon bond
- C10M137/04—Phosphate esters
- C10M137/10—Thio derivatives
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2050/00—Form in which the lubricant is applied to the material being lubricated
- C10N2050/10—Semi-solids; greasy
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Abstract
본 발명은 등속조인트용 그리이스 조성물에 관한 것으로서, 기유 68~92.8 중량%; 하기 화학식 1로 표시되는 우레아계 증주제 5~25 중량%; 몰리브덴디알킬디티오카바메이트 1.0~2.0 중량%; 아연디알킬디티오포스페이트 0.5~1.5 중량%; 유기몰리브덴착화합물 0.1~1.0 중량%; 2,5-디머캅토-1,3,4-티아디아졸 0.1~1.0 중량%; 및 유황계 지방에스터 0.5~1.5 중량%을 함유하여 이루어지는 것을 특징으로 하며,The present invention relates to a grease composition for a constant velocity joint, comprising 68 to 92.8 wt% of base oil; 5 to 25% by weight of a urea thickener represented by Formula 1; 1.0 to 2.0 wt% molybdenum dialkyldithiocarbamate; 0.5-1.5 wt.% Zinc dialkyldithiophosphate; 0.1 mol% to 1.0 wt% of an organic molybdenum complex; 0.1 to 1.0% by weight of 2,5-dimercapto-1,3,4-thiadiazole; And sulfur-based fatty esters characterized in that it comprises 0.5 to 1.5% by weight,
[화학식 1][Formula 1]
R1NH-CO-NH-C6H4-p-CH2-C6H4-p-NH-CO-NHR 2 R 1 NH-CO-NH-C 6 H 4 -p-CH 2 -C 6 H 4 -p-NH-CO-NHR 2
상기 화학식 1에서, R1과 R2는 각각 독립적으로 또는 동시에 탄소수가 6~7의 방향족 탄화수소, 또는 시클로헥실기, 또는 탄소수가 6~20의 지방족 탄화수소이다.In Formula 1, R 1 and R 2 are each independently or simultaneously an aromatic hydrocarbon having 6 to 7 carbon atoms, a cyclohexyl group, or an aliphatic hydrocarbon having 6 to 20 carbon atoms.
기유를 주재로 하고, 여기에 우레아계 증주제와 몰리브덴디알킬디티오카바메이트, 유기몰리브덴착화합물, 아연디알킬디티오포스페이트, 2,5-디머캅토-1,3,4-티아디아졸계 화합물 및 유황계 지방에스터 등의 극압첨가제 및 내마모방지제를 혼합하여 사용함으로써 내구성과 내수성이 우수해지고 극압성 및 마찰저감성이 향상되며 축력 감소 효율울 증대시키는 효과가 있다.Based on base oil, urea thickener, molybdenum dialkyldithiocarbamate, organomolybdenum complex compound, zinc dialkyldithiophosphate, 2,5-dimercapto-1,3,4-thiadiazole compound and sulfur By using extreme pressure additives such as system fat esters and anti-wear agents, the durability and water resistance are excellent, the extreme pressure and friction resistance are improved, and the axial force reduction efficiency is increased.
등속조인트, 우레아계, 리튬계, 복합리튬계, 내구성, 내수성Constant velocity joint, Urea-based, Lithium-based, Composite lithium-based, Durable, Water resistant
Description
본 발명은 등속조인트용 그리이스 조성물에 관한 것으로서, 보다 상세하게는 증주제로 우레아계(UREA)를 사용하고 극압첨가제 및 내마모방지제로 몰리브덴디알킬디티오카바메이트, 유기몰리브덴착화합물, 아연디알킬디티오포스페이트, 2,5-디머캅토-1,3,4-티아디아졸계 화합물 및 유황계 지방에스터 등을 혼합하여 사용함으로써 내구성과 내수성이 우수해지고 극압성 및 마찰저감성이 향상되며 축력 감소 효율울 증대시키는 등속조인트용 그리이스 조성물에 관한 것이다. The present invention relates to a grease composition for a constant velocity joint, and more specifically, a urea-based (UREA) as a thickener, and a molybdenum dialkyldithiocarbamate, an organic molybdenum complex compound, and a zinc dialkyldithio as an extreme pressure additive and an antiwear agent. By using phosphate, 2,5-dimercapto-1,3,4-thiadiazole-based compound, and sulfur-based fatty esters, it is excellent in durability and water resistance, improves extreme pressure and friction resistance, and improves axial force reduction efficiency. It relates to a grease composition for a constant velocity joint.
일반적으로 자동차는 엔진에서 나오는 동력이 구동축을 통해 바퀴에 전달되어 움직인다.In general, a car moves power transmitted from an engine to a wheel through a drive shaft.
이때 방향 전환을 담당하는 스티어링 휠(steering wheel)의 조작에 의해 바퀴가 좌우로 움직이는데, 이러한 움직임(동력)을 전달하는 축이 등속조인트(constant velocity joint: CVJ)이다.At this time, the wheel is moved to the left and right by the operation of the steering wheel (steering wheel) responsible for the change of direction, the axis that transmits this movement (power) is a constant velocity joint (constant velocity joint (CVJ)).
이와 같은 등속조인트는 자동차의 매우 중요한 부품으로 자동차 엔진과 바퀴 사이에 구동축으로 연결되며 바퀴가 전후 좌우 및 상하로 작동을 함에 따라 각도가 바뀌어도 엔진의 구동력을 일정한 속도로 바퀴에 전달하는 작용을 한다.Such a constant velocity joint is a very important part of a vehicle, which is connected to a driving shaft between the engine and the wheel of a vehicle, and the wheel acts to transmit the driving force of the engine to the wheel at a constant speed even when the angle changes as the wheel moves forward, backward, left, and right.
이러한 등속 조인트는 금속과 금속의 연결 부위로 이루어져 있어 금속의 마찰에 의한 마모를 방지하기 위해 접속 부위에 그리이스(GREASE)를 주입하여 고무 부트(BOOT)로 밀봉을 한다.These constant velocity joints are made of metal and metal connection parts, and in order to prevent wear due to friction of the metal, grease is injected into the connection parts and sealed with a rubber boot.
그리고 최근에는 자동차가 점점 경량화, 소형화 및 고출력화 추세로 발전하고 있으며 이에 따라 자동차 등속조인트도 소형화 되면서도 장기 수명을 요구하고 있다.In recent years, automobiles have been developed to become lighter, smaller, and higher in power, and accordingly, automotive constant velocity joints are also required to have a long life even though they are miniaturized.
따라서 자동차 등속조인트에 사용되는 그리이스는 높은 하중에서도 윤활이 가능한 극압성, 진동 및 소음을 감소시켜주는 마찰저감성도 우수하여야 하지만 자동차는 10년 이상 장기간 사용하여야 하므로 그리이스의 장기 내구성이 우수하여야 한다.Therefore, grease used in automobile constant velocity joint should be excellent in extreme pressure, which can be lubricated even under high load, and low friction which reduces vibration and noise.
또한 등속조인트의 경우 외부에 노출되어 있어서 고무 부트로 그리이스가 밀봉되어 있다 하더라도 물의 혼입이 예상되므로 물에 대한 저항력인 내수성도 우수하여야 한다.In the case of constant velocity joint, even if grease is sealed by rubber boot, water is expected to be mixed, so the water resistance, which is resistant to water, should be excellent.
그러나 종래의 등속조인트용 그리이스는 주로 극압성이나 마찰저감성을 중요한 물성으로 개발하였으나 장기 내구성 및 내수성을 고려하지 않아 수명이 단축되는 문제점이 있다. However, conventional greases for constant velocity joints have developed extreme pressure or friction resistance as important physical properties, but have a problem of shortening their lifespan without considering long-term durability and water resistance.
본 발명의 목적은 이와 같은 종래의 문제점을 해결하기 위한 것으로서, 등속조인트용 그리이스의 수명을 연장하기 위하여 증주제로 우레아계를 사용하고 5종의 극압첨가제 및 내마모방지제를 혼합하여 사용함으로써 내구성 및 내수성의 향상이 가능한 등속조인트용 그리이스 조성물을 제공하는데 있다.An object of the present invention is to solve such a conventional problem, durability and water resistance by using a urea-based as a thickener in order to extend the life of the grease for constant velocity joints and using a mixture of five extreme pressure additives and anti-wear agents It is to provide a grease composition for a constant velocity joint that can be improved.
상기한 목적을 달성하기 위한 수단으로서 본 발명의 구성은, 기유 68~92.8 중량%; 하기 화학식 1로 표시되는 우레아계 증주제 5~25 중량%; 몰리브덴디알킬디티오카바메이트 1.0~2.0 중량%; 아연디알킬디티오포스페이트 0.5~1.5 중량%; 유기몰리브덴착화합물 0.1~1.0 중량%; 2,5-디머캅토-1,3,4-티아디아졸 0.1~1.0 중량%; 및 유황계 지방에스터 0.5~1.5 중량%을 함유하여 이루어진다.As a means for achieving the above object, the configuration of the present invention, the base oil 68 ~ 92.8% by weight; 5 to 25% by weight of a urea thickener represented by Formula 1; 1.0 to 2.0 wt% molybdenum dialkyldithiocarbamate; 0.5-1.5 wt.% Zinc dialkyldithiophosphate; 0.1 mol% to 1.0 wt% of an organic molybdenum complex; 0.1 to 1.0% by weight of 2,5-dimercapto-1,3,4-thiadiazole; And 0.5 to 1.5 wt% of a sulfur-based fatty ester.
[화학식 1][Formula 1]
R1NH-CO-NH-C6H4-p-CH2-C6H4-p-NH-CO-NHR 2 R 1 NH-CO-NH-C 6 H 4 -p-CH 2 -C 6 H 4 -p-NH-CO-NHR 2
상기 화학식 1에서, R1과 R2는 각각 독립적으로 또는 동시에 탄소수가 6~7의 방향족 탄화수소, 또는 시클로헥실기, 또는 탄소수가 6~20의 지방족 탄화수소이다.In Formula 1, R 1 and R 2 are each independently or simultaneously an aromatic hydrocarbon having 6 to 7 carbon atoms, a cyclohexyl group, or an aliphatic hydrocarbon having 6 to 20 carbon atoms.
본 발명의 그리이스 조성물은 기유를 주재로 하여, 리튬계(LITHIUM) 증주제, 복합리튬계(LITHIUM COMPLEX) 증주제, 우레아계 증주제를 비교 시험하였고, 여기에 5종 이상의 극압첨가제 및 내마모방지제를 포함한다.The grease composition of the present invention was based on a base oil, and was tested for a lithium-based (LITHIUM) thickener, a lithium-based (LITHIUM COMPLEX) thickener, and a urea-based thickener, and includes five or more extreme pressure additives and anti-wear agents. .
상기 기유는 정제된 파라핀계 광유를 사용하며 상기 정제된 파라핀계 광유는 100℃에서의 동점도는 8~12cSt이고 40℃에서의 동점도는 90~120cSt인 것을 특징으로 한다.The base oil is a purified paraffinic mineral oil and the purified paraffinic mineral oil is characterized in that the kinematic viscosity at 100 ℃ is 8 ~ 12cSt and the kinematic viscosity at 40 ℃ is 90 ~ 120cSt.
본 발명은 그리이스 증주제로서 리튬계, 복합리튬계, 우레아계 증주제를 비 교 시험한 결과 내구성 및 내수성이 우수한 그리이스를 제조하게 되어 본 발명을 완성하였다.The present invention is a grease thickener as a result of comparing the lithium-based, composite lithium-based, urea-based thickener as a result of producing a grease excellent in durability and water resistance to complete the present invention.
이러한 본 발명의 내구성 및 내수성이 우수한 그리이스 조성물은 자동차의 등속조인트용 그리이스로 사용이 가능하다.The grease composition having excellent durability and water resistance of the present invention can be used as a grease for a constant velocity joint of an automobile.
이러한 본 발명의 증주제는 하기 화학식 1~3으로 표시되는 우레아계 증주제, 리튬계 증주제, 복합리튬계 증주제를 사용한다.The thickener of the present invention uses a urea-based thickener, a lithium-based thickener, and a composite lithium-based thickener represented by the following Chemical Formulas 1-3.
[화학식 1][Formula 1]
R1NH-CO-NH-C6H4-p-CH2-C6H4-p-NH-CO-NHR 2 R 1 NH-CO-NH-C 6 H 4 -p-CH 2 -C 6 H 4 -p-NH-CO-NHR 2
[화학식 2][Formula 2]
[화학식 3][Formula 3]
상기 화학식 1에서, R1과 R2는 각각 독립적으로 또는 동시에 탄소수가 6~7의 방향족 탄화수소, 또는 시클로헥실기, 또는 탄소수가 6~20의 지방족 탄화수소이다.In Formula 1, R 1 and R 2 are each independently or simultaneously an aromatic hydrocarbon having 6 to 7 carbon atoms, a cyclohexyl group, or an aliphatic hydrocarbon having 6 to 20 carbon atoms.
상기 화학식 1의 우레아 증주제는 디이소시아네이트와 2당량의 알킬아민 또는 시클로아민 또는 아릴아민을 윤활기유 존재하에서 반응시켜 제조할 수 있다.The urea thickener of Chemical Formula 1 may be prepared by reacting diisocyanate with 2 equivalents of alkylamine or cycloamine or arylamine in the presence of a lubricant base oil.
이때 디이소시아네이트는 4,4-메틸렌비스(페닐이소시아네이트)를 사용하는 것이 바람직하며, 아릴아민으로는 탄소수가 6~7개인 방향족아민 또는 시클로아민으로는 시클로헥실아민 또는 알킬아민으로는 탄소수가 6~20개인 지방족아민을 사용하는 것이 바람직하다.In this case, it is preferable to use 4,4-methylenebis (phenylisocyanate) as the diisocyanate, and aromatic amine having 6 to 7 carbon atoms as arylamine or cyclohexylamine as cycloamine or 6 to carbon atoms as alkylamine. Preference is given to using 20 aliphatic amines.
상기 우레아계 증주제의 사용함량은 전체 조성물에 대하여 5~25 중량%인 것이 바람직하며, 이때 증주제 함량이 5중량% 미만이면 주도가 묽어져서 내구성이 떨어지고 25중량%를 초과하면 주도가 되어져서 윤활성 및 저온성이 나빠지는 문제점이 있다.The use amount of the urea-based thickener is preferably 5 to 25% by weight based on the total composition, wherein when the thickener content is less than 5% by weight, the led is diluted and the durability is lowered. There is a problem that the low temperature worsens.
상기 화학식 2의 리튬계 증주제는 12-히드록시스테아린산과 수산화리튬을 반응시켜 제조할 수 있다.The lithium thickener of Chemical Formula 2 may be prepared by reacting 12-hydroxystearic acid with lithium hydroxide.
이때 12-히드록시스테아린산은 탄소수 18개인 지방산을 사용하며, 수산화리튬은 순도 57%를 사용하는 것이 바람직하다.At this time, 12-hydroxystearic acid uses a fatty acid having 18 carbon atoms, lithium hydroxide is preferably 57% purity.
상기 리튬계 증주제의 함량은 5~13 중량%을 사용하는 것이 바람직하며 증주제 함량이 5% 이하는 그리이스가 묽어지고 13% 이상은 되어진다.The content of the lithium thickener is preferably 5 to 13% by weight, and the thickener is less than 5% grease is diluted and 13% or more.
상기 화학식 3의 복합리튬계 증주제는 12-히드록시스테아린산과 2당량의 아젤라인산과 수산화리튬을 반응시켜 제조할 수 있다.The composite lithium thickener of Chemical Formula 3 may be prepared by reacting 12-hydroxystearic acid with 2 equivalents of azelaic acid and lithium hydroxide.
이때 12-히드록시스테아린산은 탄소수 18개인 지방산을 사용하며, 아젤라인산은 탄소수 9개인 지방산을 사용하고 수산화리튬은 순도 57%를 사용하는 것이 바람직하다.In this case, it is preferable that 12-hydroxystearic acid uses a fatty acid having 18 carbon atoms, azelaic acid uses a fatty acid having 9 carbon atoms, and lithium hydroxide has a purity of 57%.
상기 복합리튬계 증주제의 함량은 8~18 중량%을 사용하는 것이 바람직하며 증주제 함량이 8% 이하면 그리이스가 묽어지고 18% 이상이면 되어진다.The content of the composite lithium thickener is preferably 8 to 18% by weight. If the thickener content is 8% or less, the grease may be diluted and 18% or more.
또한 본 발명은 5종의 극압첨가제 및 내마모장지제를 혼합하여 사용한다.In addition, the present invention uses a mixture of five extreme pressure additives and abrasion resistance.
상기 첨가제로는 몰리브덴 디알킬디티오카바메이트, 아연 디알킬디티오포스페이트, 유기 몰리브덴 착화합물, 2,5-디머캅토-1,3,4-티아디아졸, 및 유황계 지방에스터를 사용하는 것이 바람직하다.As the additive, it is preferable to use molybdenum dialkyldithiocarbamate, zinc dialkyldithiophosphate, organic molybdenum complex compound, 2,5-dimercapto-1,3,4-thiadiazole, and sulfur-based fatty ester. Do.
그리고 본 발명은 상기에서 언급한 우레아계 증주제 2종을 제조하였다.In the present invention, two kinds of urea thickeners mentioned above were prepared.
1종은 지방족아민과 지환족아민 또는 방향족아민을 사용하였으며, 2종은 지환족아민과 방향족아민을 사용하였다.One used aliphatic amine and alicyclic amine or aromatic amine, and the other used alicyclic amine and aromatic amine.
여기서 후자의 것이 내구성 즉 전단안정성 면이 우수하게 나타내었다.The latter one showed excellent durability, that is, shear stability.
그리이스의 극압성 및 마찰저감성을 유지하면서 장기 내구성을 향상시키는 것은 증주제이며 상기 증주제의 전단안정성 비교를 통하여 내구성이 우수한 등속조인트용 그리이스 조성물을 개발하였다.Improving long-term durability while maintaining the extreme pressure and friction resistance of the grease is a thickener and through the comparison of the shear stability of the thickener was developed a grease composition for constant velocity joints excellent durability.
또한, 본 발명의 그리이스 조성물은 필요에 따라 적절한 다른 첨가제를 포함할 수 있다.In addition, the grease composition of the present invention may include other additives as appropriate.
예를 들면, 본 발명의 그리이스 조성물은 아민계 산화방지제 0.5~1.0 중량%, 동판부식방지제인 중성바륨디노닐설포네이트 0.1~0.5 중량%를 사용할 수 있다.For example, the grease composition of the present invention may use 0.5 to 1.0% by weight of an amine antioxidant, 0.1 to 0.5% by weight of neutral barium dinonylsulfonate as a copper corrosion inhibitor.
본 발명은 다음의 비교예를 통하여 더욱 상세하게 설명될 것이다.The invention will be explained in more detail by the following comparative examples.
비교예 1Comparative Example 1
온도계, 적하깔대기, 교반기가 장착된 2L 그리이스 반응기에 100℃에서 동점도가 8~12 cSt인 윤활기유 720g과 12-히드록시스테아린산 180g을 가하고 70~110℃로 가열하여 10~30분간 교반한다.In a 2L grease reactor equipped with a thermometer, a dropping funnel and a stirrer, 720 g of lubricating base oil having a kinematic viscosity of 8 to 12 cSt and 180 g of 12-hydroxystearic acid were added at 100 ° C., and the mixture was heated to 70 to 110 ° C. and stirred for 10 to 30 minutes.
내용물이 완전히 용해되면 수산화리튬 25g을 서서히 가하고 100~140℃에서 교반하면서 검화반응시킨다.When the contents are completely dissolved, 25 g of lithium hydroxide is slowly added and saponified while stirring at 100 to 140 ° C.
반응이 대부분 완료되면 반응기 내부의 온도를 140~160℃로 승온하여 중간오일 500g을 투입하고 교반한다.When most of the reaction is completed, the temperature inside the reactor is raised to 140 ~ 160 ℃ to add 500g of intermediate oil and stirred.
반응기 내부의 온도를 190~200℃로 승온하여 10~30분간 교반하면서 온도를 유지한 후 냉각오일 400g을 투입하고 충분히 교반하면서 냉각시킨다.The temperature inside the reactor was raised to 190-200 ° C. and the temperature was maintained while stirring for 10-30 minutes. Then, 400 g of cooling oil was added thereto and cooled with sufficient stirring.
반응기 내부의 온도가 130~150℃ 전후로 냉각되면 극압제 및 마찰저감제로 몰리브덴디알킬디티오카바메이트 1.5 중량%, 아연디알킬디티오포스페이트 1.5 중량%, 유기몰리브덴착화합물 1.0 중량%, 2,5-디머캅토-1,3,4-티아디아졸 1.0 중량%을 첨가하였으며 기타 첨가제로 아민계 산화방지제 0.5 중량%, 동판부식방지제인 중성바륨디노닐설포네이트 0.5 중량%를 첨가한 후 10~30분간 추가로 교반하면서 윤활기유를 조금씩 가하여 그리이스의 혼화주도를 300 전후로 조절하였으며, 제조가 완료되면 콜로이드밀로 균질화 처리를 하여 그리이스를 제조하였다.When the temperature inside the reactor is cooled to around 130-150 ° C, 1.5% by weight of molybdenum dialkyldithiocarbamate, 1.5% by weight of zinc dialkyldithiophosphate, 1.0% by weight of organo-molybdenum complex compound, as extreme pressure and friction reducing agent 1.0% by weight of dimercapto-1,3,4-thiadiazole was added, and then 0.5% by weight of amine antioxidant and 0.5% by weight of neutral barium dinonylsulfonate as a copper corrosion inhibitor were added as other additives. Grease base oil was added little by little while stirring, and the mixing direction of grease was adjusted to around 300. When the preparation was completed, the grease was prepared by homogenizing with a colloid mill.
비교예 2Comparative Example 2
온도계, 적하깔대기, 교반기가 장착된 2L 그리이스 반응기에 100℃에서 동점도가 8~12 cSt인 윤활기유 850g과 12-히드록시스테아린산 180g을 가하고 70~110℃로 가열하여 10~30분간 교반한다.In a 2L grease reactor equipped with a thermometer, a dropping funnel and a stirrer, 850 g of lubricating base oil having a kinematic viscosity of 8 to 12 cSt and 180 g of 12-hydroxystearic acid at 100 ° C. are heated to 70 to 110 ° C. and stirred for 10 to 30 minutes.
내용물이 완전히 용해되면 수산화리튬 25g을 서서히 가하고 80~120℃에서 교반하면서 검화반응시킨다.When the contents are completely dissolved, 25 g of lithium hydroxide is slowly added and saponified while stirring at 80 to 120 ° C.
반응이 대부분 완료되면 아젤라인산 90g을 투입하여 용해하고 수산화리튬 40g을 서서히 가하고 80~120℃에서 검화반응시킨다.When most of the reaction is completed, 90 g of azelaic acid is added to dissolve the solution, and 40 g of lithium hydroxide is slowly added thereto, followed by saponification at 80 to 120 ° C.
반응기 내부의 온도를 190~210℃로 승온하여 10~30분간 교반하면서 온도를 유지한 후 냉각오일 300g을 투입하고 충분히 교반하면서 냉각시킨다.The temperature inside the reactor was raised to 190-210 ° C., the temperature was maintained while stirring for 10-30 minutes, and 300 g of cooling oil was added thereto, followed by cooling with sufficient stirring.
첨가제는 비교예 1과 동일하게 첨가하였다.The additive was added in the same manner as in Comparative Example 1.
실시예 1Example 1
온도계, 적하깔때기, 교반기가 장착된 2L 그리이스 반응기에 100℃에서 동점도가 8~12 cSt인 윤활기유 400g과 4,4-메틸렌비스(페닐이소시아네이트) 114g을 가하고 70~110℃로 가열하여 10~30분간 교반한다.To a 2L grease reactor equipped with a thermometer, a dropping funnel and a stirrer, 400 g of lubricating base oil having a kinematic viscosity of 8 to 12 cSt and 114 g of 4,4-methylenebis (phenylisocyanate) at 100 ° C. were heated to 70 to 110 ° C., and then to 10 to 30. Stir for minutes.
내용물이 완전히 용해되면 시클로헥실아민 70g과 지방족아민 70g을 가하고 80~120℃에서 교반하면서 반응시킨다.When the contents are completely dissolved, add 70 g of cyclohexylamine and 70 g of aliphatic amine and react with stirring at 80 ~ 120 ℃.
반응이 대부분 완료되면 반응기 내부의 온도를 140~160℃로 승온하여 20분 이상 충분히 교반하면서 반응시킨다.When the reaction is mostly completed, the temperature inside the reactor is raised to 140-160 ° C. and reacted with sufficient stirring for 20 minutes or more.
반응 내용물에 윤활기유 100g을 추가로 가하고 반응기 내부의 온도를 190~210℃로 승온시킨다.100 g of lubricating base oil is further added to the reaction contents, and the temperature inside the reactor is raised to 190 to 210 ° C.
상기 온도에서 약 10분간 교반한 후 나머지 윤활기유 200g을 가하고 교반하면서 냉각시킨다.After stirring for about 10 minutes at the temperature, 200g of the remaining lubricant base oil is added and cooled with stirring.
반응기 내부의 온도가 100℃ 전후로 냉각되면 극압제 및 마찰저감제로 몰리브덴디알킬디티오카바메이트 1.5 중량%, 아연디알킬디티오포스페이트 1.5 중량%, 유가몰리브덴착화합물 1.0 중량%, 2,5-디머캅토-1,2,4-티아디아졸계 화합물 1.0 중량%를 첨가하였으며 기타 첨가제로 아민계 산화방지제 0.5 중량%, 동판부식방지제 인 중성바륨디노닐설포네이트 0.5 중량%를 첨가한 후 10~30분간 추가로 교반하면서 윤활기유를 조금씩 가하여 그리이스의 혼화주도를 300 전후로 조절하였으며, 제조가 완료되면 콜로이드밀로 균질화 처리를 하여 그리이스를 제조하였다.When the temperature inside the reactor is cooled to around 100 ° C, 1.5% by weight of molybdenum dialkyldithiocarbamate, 1.5% by weight of zinc dialkyldithiophosphate, 1.0% by weight of a molybdenum complex compound and 2,5-dimercapto are used as extreme pressure and friction reducing agents. 1.0 wt% of -1,2,4-thiadiazole-based compound was added, and 0.5 wt% of amine antioxidant and 0.5 wt% of neutral barium dinonylsulfonate as copper corrosion inhibitor were added as other additives. Grease base oil was added little by little with stirring to adjust the blending orientation of the grease to around 300. When the preparation was completed, the grease was prepared by homogenizing with a colloid mill.
실시예 2Example 2
실시예 1의 방법과 동일하게 제조하였으며 지방족아민 대신 방향족아민을 사용하였다.The preparation was carried out in the same manner as in Example 1, and aromatic amines were used instead of aliphatic amines.
첨가제도 실시예 1과 동일하게 첨가하였다.An additive was also added in the same manner as in Example 1.
상기한 비교예 1~2와 실시예 1~2의 성상을 다음 표 1에 나타내었다.The properties of the above Comparative Examples 1-2 and Examples 1-2 are shown in Table 1 below.
실험예 1Experimental Example 1
비교예 1~2와 실시예 1~2의 전단안정성을 비교하기 위하여 혼화안정도를 실시하였다.In order to compare the shear stability of Comparative Examples 1 and 2 and Examples 1 and 2 were mixed stability.
혼화안정도 시험은 ASTM D 217의 방법에 따라 실시하였다.The miscibility test was performed according to the method of ASTM D 217.
좀 더 자세히 설명하면 그리이스가 장시간 기계적인 사용에 따라 묽어지는 정도를 측정하는 시험으로 혼화안정도기를 사용하여 그리이스 컵에 시료를 채운 후 10만회 왕복시킨 후 25℃에서 주도를 측정하는 시험이다.In more detail, it is a test to measure the degree of grease dilution according to the mechanical use for a long time. It is a test to measure the lead at 25 ° C after filling the grease cup with a sample using a mixed stabilizer, and then reciprocating 100,000 times.
혼화전의 주도와 혼화후의 주도의 차이로 측정하는데 차이가 작을 수록 혼화안정도 즉 전단안정성이 우수하다.The smaller the difference, the better the stability of mixing, that is, shear stability.
위의 표 1에 나타낸 비교예 1~2와 실시예 1~2의 혼화안정도를 다음 표 2에 나타내었다.The mixing stability of Comparative Examples 1 and 2 and Examples 1 and 2 shown in Table 1 above is shown in Table 2 below.
실험예 2Experimental Example 2
비교예 1~2와 실시예 1~2의 물의 혼입 시의 전단안정성을 비교하기 위하여 수혼화안정도를 실시하였다.In order to compare the shear stability at the time of mixing water of Comparative Examples 1 and 2 and Examples 1 and 2, water miscibility was performed.
시험은 실험예 1과 동일하고 시료에 10%의 물을 투입한다.The test is the same as in Experiment 1 and 10% of water is added to the sample.
위의 표 1에 나타낸 비교예 1~2와 실시예 1~2의 수혼화안정도를 다음 표 3에 나타내었다.The water miscibility stability of Comparative Examples 1 and 2 and Examples 1 and 2 shown in Table 1 above is shown in Table 3 below.
상기 표 2~3의 결과에서 보면, 비교예 1의 경우 혼화안정도는 ±40정도 묽어졌으나 수혼화안정도에서는 +110정도로 매우 많이 묽어졌으며, 비교예 2의 경우 혼화안정도는 ±26정도 묽어졌고 수혼화안정도는 +50정도 묽어졌다.In the results of Tables 2 to 3, in the case of Comparative Example 1, the miscibility was diluted about ± 40, but in the water-miscibility stability, it was very much diluted to about +110, and in the case of Comparative Example 2, the miscibility was about ± 26 and the water-miscible Stability was diluted by +50.
실시예 1의 경우 혼화안정도가 ±40정도 묽어졌고 수혼화안정도는 +41정도 묽어졌으며, 실시예 2의 경우 혼화안정도가 +20정도 묽어졌고 수혼화안정도는 +28 정도 묽어졌다.In Example 1, the miscibility was about ± 40 and the water miscibility was about +41. In Example 2, the miscibility was about +20 and the water miscibility was about +28.
비교예 1~2와 실시예 1~2에서 혼화안정도의 경우 실시예 2가 가장 우수하며 수혼화안정도는 비교예 1이 가장 많이 묽어졌다.In Comparative Examples 1 and 2 and Examples 1 and 2, Example 2 was the most excellent, and in the water mixing stability, Comparative Example 1 was the most diluted.
실시예 1~2는 수혼화안정도에서 비교예 1~2보다 우수하다.Examples 1-2 are superior to Comparative Examples 1-2 in the water-miscibility stability.
더 상세히 설명하면 수분의 환경조건에서는 우레아 증주제 그리이스가 다른 리튬계 증주제나 복합리튬계 증주제보다 우수하게 나타났으며 우레아 증주제의 종류에 따라서도 혼화안정도가 차이가 나타났다.In detail, the urea thickener grease was superior to other lithium type thickeners or composite lithium type thickeners in the environmental conditions of moisture, and miscibility was also different according to the type of urea thickener.
실험예 3Experimental Example 3
비교예 1~2와 실험예 1~2의 전단아정성을 측정하기 위해 롤스테빌러티를 실시하였다.In order to measure the shear stability of Comparative Examples 1-2 and Experimental Examples 1-2, roll stability was performed.
시험 방법은 ASTM D 1831에 따라 실시하였다.The test method was conducted according to ASTM D 1831.
롤스테빌러티는 원통안에 시료를 50g 정도 채운 후 상온에서 165rpm으로 2시간 가동시킨 후의 주도를 측정한다.Roll Stability measures the ledness after filling about 50g of sample in the cylinder and operating it for 2 hours at 165rpm at room temperature.
좀더 상세히 설명하면 두 물체가 접촉하여 작동시 윤활 역할을 하는 그리이스의 묽어지는 정도를 나타낸다.In more detail, the degree of grease dilution, which is the lubrication of the two objects in contact and operation, is shown.
롤 전의 주도와 롤 후의 주도의 차이로 측정하는데 차이가 작을 수록 롤스테빌러티 즉 기계적인 전당안정성이 우수하다.It is measured by the difference between the lead before the roll and the lead after the roll. The smaller the difference, the better the roll stability, that is, the mechanical hall stability.
위의 표 1에 수록된 비교예 1~2와 실시예 1~2의 롤스테빌러티를 다음 표 4에 나타내었다.Roll Stability of Comparative Examples 1 and 2 and Examples 1 and 2 listed in Table 1 above are shown in Table 4 below.
상기 표 4의 결과를 살펴보면, 본 발명에서 제조한 실시예 4의 경우 롤 안정도가 가장 우수하게 나타났으며 비교예 1이 가장 나쁘게 나타났다.Looking at the results of Table 4, in the case of Example 4 prepared in the present invention, roll stability was most excellent and Comparative Example 1 was the worst.
앞에서도 언급한 것처럼 실시예 1~2의 경우 우레아 증주제의 종류에 따라서도 전단안정성이 차이가 나타났다.As mentioned above, in Examples 1 and 2, shear stability was also different depending on the type of urea thickener.
이상에서 설명한 바와 같이, 본 발명의 실시예에 따른 등속조인트용 그리이스 조성물은 기유를 주재로 하고, 여기에 우레아계 증주제와 몰리브덴디알킬디티오카바메이트, 유기몰리브덴착화합물, 아연디알킬디티오포스페이트, 2,5-디머캅토-1,3,4-티아디아졸계 화합물 및 유황계 지방에스터 등의 극압첨가제 및 내마모방지제를 혼합하여 사용함으로써 내구성과 내수성이 우수해지고 극압성 및 마찰저감성이 향상되며 축력 감소 효율울 증대시키는 효과를 얻을 수 있다.As described above, the grease composition for the constant velocity joint according to the embodiment of the present invention is based on a base oil, wherein a urea thickener, a molybdenum dialkyl dithio carbamate, an organic molybdenum complex compound, a zinc dialkyl dithio phosphate, By using extreme pressure additives and anti-wear agents such as 2,5-dimercapto-1,3,4-thiadiazole-based compounds and sulfur-based fatty esters, they have excellent durability and water resistance, and improve extreme pressure and friction reduction. The effect of increasing the axial force reduction efficiency can be obtained.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR100828176B1 (en) | 2006-12-29 | 2008-05-08 | 한국프랜지공업 주식회사 | Grease composition having high durability and low friction force for constant velocity joints |
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|---|---|---|---|---|
| JPH04279698A (en) * | 1991-03-07 | 1992-10-05 | Nippon Oil Co Ltd | Grease composition for synchromesh joint |
| US6037314A (en) | 1996-06-07 | 2000-03-14 | Kyodo Yushi Co., Ltd. | Grease composition for constant velocity joints |
| KR20000043997A (en) * | 1998-12-29 | 2000-07-15 | 정몽규 | Grease composition with high pressure resistance and wear-resistance |
| KR100541148B1 (en) * | 2003-09-29 | 2006-01-11 | 한국프랜지공업 주식회사 | Grease composition for automobile constant velocity joints |
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- 2004-12-01 KR KR1020040099944A patent/KR100562129B1/en active IP Right Grant
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04279698A (en) * | 1991-03-07 | 1992-10-05 | Nippon Oil Co Ltd | Grease composition for synchromesh joint |
| US6037314A (en) | 1996-06-07 | 2000-03-14 | Kyodo Yushi Co., Ltd. | Grease composition for constant velocity joints |
| KR20000043997A (en) * | 1998-12-29 | 2000-07-15 | 정몽규 | Grease composition with high pressure resistance and wear-resistance |
| KR100541148B1 (en) * | 2003-09-29 | 2006-01-11 | 한국프랜지공업 주식회사 | Grease composition for automobile constant velocity joints |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100828176B1 (en) | 2006-12-29 | 2008-05-08 | 한국프랜지공업 주식회사 | Grease composition having high durability and low friction force for constant velocity joints |
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