KR20020083754A - Grease composite of extreme pressure and wear preventive characteristics - Google Patents

Grease composite of extreme pressure and wear preventive characteristics Download PDF

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KR20020083754A
KR20020083754A KR1020010023372A KR20010023372A KR20020083754A KR 20020083754 A KR20020083754 A KR 20020083754A KR 1020010023372 A KR1020010023372 A KR 1020010023372A KR 20010023372 A KR20010023372 A KR 20010023372A KR 20020083754 A KR20020083754 A KR 20020083754A
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extreme pressure
grease composition
sulfur
compound
group
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KR1020010023372A
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Korean (ko)
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나기식
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현대자동차주식회사
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Publication of KR20020083754A publication Critical patent/KR20020083754A/en

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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
    • C10M135/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing sulfur, selenium or tellurium
    • C10M135/12—Thio-acids; Thiocyanates; Derivatives thereof
    • C10M135/14—Thio-acids; Thiocyanates; Derivatives thereof having a carbon-to-sulfur double bond
    • C10M135/18—Thio-acids; Thiocyanates; Derivatives thereof having a carbon-to-sulfur double bond thiocarbamic type, e.g. containing the groups
    • 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
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
    • 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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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Lubricants (AREA)

Abstract

PURPOSE: Provided is an extreme pressure(EP) grease composition having abrasion resistance, which comprises base oil having increased extreme pressure property and abrasion resistance, organic compound, and extreme pressure additive, wherein the content of sulfur and phosphorus components is 0.5-3 wt%. CONSTITUTION: The grease composition consists of base oil, organic compound and extreme pressure additive. Also, the composition comprises 0.5-10 wt% of organic molybdenum compound and 0.5-10 wt% of extreme additive, wherein the content of sulfur and phosphorus components is 0.5-3 wt%. The organic molybdenum compound is an organic compound which does not contain sulfur, or a molybdenum-sulfur complex. The organic molybdenum compound is represented by formula 1: ((R-O)n(HO)3-nPO)(MoO3)x(wherein x is an integer of 1-7 when n is 1, x is an integer of 1-6 when n is 2, R is hydrocarbyl group, alkyl group, aryl group, aralkyl group, cycloalkyl group or alkaryl group).

Description

극압 및 내마모성 그리스 조성물{Grease composite of extreme pressure and wear preventive characteristics}Grease composite of extreme pressure and wear preventive characteristics

본 발명은 극압 및 내마모성 그리스 조성물에 관한 것으로서, 더욱 상세하게는 종래 그리스 조성물 중에 유기 몰리브덴 화합물과 극압첨가제를 혼합 첨가하여 전체 그리스 조성 중의 유황 및 인 성분의 함량을 일정범위로 제한함으로써, 극압성과 내마모성을 향상시킨 극압 및 내마모성 그리스 조성물에 관한 것이다.The present invention relates to an extreme pressure and wear resistant grease composition, and more particularly, by adding an organic molybdenum compound and an extreme pressure additive in a conventional grease composition to limit the content of sulfur and phosphorus in the total grease composition to a certain range, thereby providing extreme pressure and wear resistance The present invention relates to an extreme pressure and wear resistant grease composition having improved pressure.

일반적으로 종래에는 극압이 걸림으로 말미암아 마모가 쉽게 일어나는 윤활 부위로서 자동차의 유니버설 조인트, 스프라인 샤프트, 변속기어, 산업용 기계의 기어카프링 등과 같은 부위에 유황-인계 극압첨가제를 함유한 그리스, 또는 이황화몰리브덴을 함유한 극압 그리스 또는 유기몰리브덴-아연 화합물을 함유하는 그리스 조성물을 사용하고 있다.In general, grease containing sulfur-phosphorus extreme pressure additives in parts such as universal joints, spline shafts, transmission gears, and gear couplings of industrial machines, etc., is a lubrication part that is easily worn due to extreme pressure. A grease composition containing an extreme pressure grease or an organomolybdenum-zinc compound containing is used.

이러한 종래의 그리스 조성물은 마모방지제로서 잰트에이트계(Xanthates) 구조를 갖는 XAN 또는 R2XAN으로 표시되는 디티오카보네이트와 디티오카바메이트(예를들면 Mo-DTC), 디티오포스페이트계(예를 들면 Mo-DTP), 디케톤계(예를 들면 Mo2S4[CH3C(O)CHCOCH3-]2), 디티오레이트계(예를 들면 Mo-(TDT)2, TDT=톨루엔-3,4-디티올), 디머캅토 티아디아졸계(예를 들면 Mo-(DMT)2, DMT=2,5 디머캅토-1,3,4-티아디아졸) 등의 유황이 포함된 유기 몰리브덴 화합물을 첨가하여 사용하여 왔다. 그러나, 상기와 같이 유황-인계 극압첨가제를 함유한 그리스나 이황화몰리브덴을 함유한 극압 그리스 또는 유기몰리브덴-아연 화합물을 함유한 그리스는 가혹한 윤활 조건의 경우 윤활면에 오일이 쉽게 침투하기 어려워 마모가 발생하는 문제점이 있다. 특히, 유황-인계 첨가제를 사용하는 경우 극압을 향상시키고 마모계수를 낮추기 위해서 비교적 다량의 첨가제를 사용해야 하며, 이때 유황-인계 화합물이 고온에서 분해될 때 생기는 활성 유황에 의한 그리스의 열화나 산성 화합물에 의한 부식 및 마모문제가 발생하였다.Such conventional grease compositions include dithiocarbonate, dithiocarbamate (e.g. Mo-DTC), dithiophosphate type (e.g., XAN or R 2 XAN having a xanthates structure as an antiwear agent). Mo-DTP), diketones (eg Mo 2 S 4 [CH 3 C (O) CHCOCH 3- ] 2 ), dithiolates (eg Mo- (TDT) 2 , TDT = toluene-3 Organic molybdenum compounds containing sulfur such as (4-dithiol) and dimercapto thiadiazole (for example, Mo- (DMT) 2 , DMT = 2,5 dimercapto-1,3,4-thiadiazole) Has been used. However, as described above, grease containing sulfur-based extreme pressure additives or extreme pressure greases containing molybdenum disulfide or greases containing organomolybdenum-zinc compounds are difficult to penetrate into the lubricating surface under severe lubrication conditions, causing wear. There is a problem. In particular, when using sulfur-based additives, a relatively large amount of additives should be used to improve the extreme pressure and lower the wear coefficient. Corrosion and wear problems occurred.

이밖에도 유기 몰리브덴 화합물, 즉 몰리브덴 디티오카바메이트(DTC0와 몰리브덴 디티오포스페이트계(DTP)를 단독 또는 병용하여 사용하는 경우는 유황 원자를 포함하고 있는 유기 몰리브덴이 분해될 때 생기는 이황화몰리브덴 화합물에 의한 부식 및 마모가 여전히 발생하여 이를 해결해야 할 필요성이 절실히 요구되는 실정이었다.In addition, when the organic molybdenum compound, ie, molybdenum dithiocarbamate (DTC0 and molybdenum dithiophosphate system (DTP), alone or in combination) is used, corrosion of the molybdenum disulfide compound generated when the organic molybdenum containing sulfur atoms is decomposed And abrasion still occurs, the need to solve this situation is urgently needed.

이에, 본 발명의 별명자는 상기 종래와 같은 문제점을 해결하기 위하여 예의노력한 결과, 종래의 그리스 조성물 중에 유기 몰리브덴 화합물과 극압첨가제를 첨가하되 전체 그리스 조성 중의 유황 및 인 성분의 함량을 3 중량% 이내로 제한하면 그리스의 내마모성과 극압성을 향상시킬 수 있음을 확인함으로써, 본 발명을 완성하였다.Thus, the nickname of the present invention is an effort to solve the problems as described above, as a result, adding the organic molybdenum compound and the extreme pressure additive in the conventional grease composition, while limiting the content of sulfur and phosphorus components in the total grease composition within 3% by weight The present invention was completed by confirming that the grease abrasion resistance and extreme pressure resistance could be improved.

결국, 본 발명의 주된 목적은 극압 및 내마모성이 향상된 기유, 유기화합물 및 극압첨가제를 포함하되, 전체 그리스 조성 중 유황 및 인 성분의 함량이 0.5 ∼ 3 중량%인 것을 특징으로 하는 그리스 조성물을 제공하는 데 있다.After all, the main object of the present invention is to provide a grease composition comprising a base oil, an organic compound and an extreme pressure additive with improved extreme pressure and wear resistance, the content of sulfur and phosphorus in the total grease composition is 0.5 to 3% by weight There is.

본 발명은 기유, 유기화합물 및 극압첨가제로 이루어진 그리스 조성물에 있어서, 상기 그리스 조성물 중에 유기 몰리브덴 화합물 0.5 ∼ 10 중량% 및 극압첨가제 0.5 ∼ 10 중량%를 포함하되, 전체 그리스 조성물 중에 유황 및 인 성분의 함량이 0.5 ∼ 3 중량%인 극압 및 내마모성 그리스 조성물을 그 특징으로 한다.The present invention relates to a grease composition comprising a base oil, an organic compound and an extreme pressure additive, wherein the grease composition contains 0.5 to 10 wt% of an organic molybdenum compound and 0.5 to 10 wt% of an extreme pressure additive, It is characterized by extreme pressure and wear resistant grease compositions with a content of 0.5 to 3% by weight.

이하, 본 발명을 더욱 상세히 설명하면 다음과 같다.Hereinafter, the present invention will be described in more detail.

본 발명의 그리스 조성물은 기유를 기재로 하여, 유기 화합물 중 유기 몰리브덴 화합물과 극압첨가제를 동시에 혼합 사용하고, 조성물 중의 유황 및 인 성분의 함량을 일정범위로 유지하는데 그 특징이 있다.The grease composition of the present invention is characterized by using an organic molybdenum compound and an extreme pressure additive in an organic compound at the same time, and maintaining the sulfur and phosphorus content in the composition in a certain range.

본 발명에서 사용되는 유기 몰리브덴 화합물로는 유황이 함유되어 있지 않은 유기 몰리브덴 화합물 또는 몰리브덴-유황(Mo-S) 복합체를 사용하는 것이 바람직하다. 상기 유황이 함유되어 있지 않은 유기몰리브덴 화합물로는 인과 산소를 포함하고 있는 다음 화학식 1로 표시되는 화합물을 사용하는 것이 바람직하다.As the organic molybdenum compound used in the present invention, it is preferable to use an organic molybdenum compound or a molybdenum-sulfur (Mo-S) composite containing no sulfur. As the organic molybdenum compound containing no sulfur, it is preferable to use a compound represented by the following formula (1) containing phosphorus and oxygen.

상기 화학식 1에서, n은 1일 때 x는 1 ∼ 7의 정수이고, n은 2일 때 x는 1 ∼ 6의 정수이고, R은 하이드로카빌기, 알킬기, 아릴기, 알알킬기(aralkyl), 사이클로알킬기 또는 알카릴기(alkaryl)이다.In Formula 1, when n is 1, x is an integer of 1 to 7, when n is 2, x is an integer of 1 to 6, R is a hydrocarbyl group, an alkyl group, an aryl group, an alalkyl group, Cycloalkyl group or alkaryl group.

이러한 화합물의 구체적인 예를 들면, 시판되는 반데르빌트(Vanderbilt)사의 제품 몰리반(Molyvan) 855 또는 몰리반(Molyvan) 856이 있다. 상기 유기 몰리브덴 화합물의 사용량은 0.5 ∼ 10 중량%로 사용하며, 이때 유기 몰리브덴 화합물의 함량이 상기 범위를 벗어나면 마모성이 불리해지는 문제점이 있게 된다.Specific examples of such compounds are the commercially available Vanderbilt product Molyvan 855 or Molyvan 856. The amount of the organic molybdenum compound is used in an amount of 0.5 to 10% by weight. At this time, when the content of the organic molybdenum compound is outside the above range, there is a problem in that wearability is disadvantageous.

또한, 상기 극압첨가제로는 유황-인계 첨가제로서 산화방지 효과가 큰 식물성 황화유지, 광물성 황화유지, 납티아밀 디티오카바메이트, 안티몬 디알킬디티오카바메이트, 및 안티몬 디알킬 포스포로 디티오에이트 중에서 선택되는 1종 또는 2종의 혼합물을 사용하는 것이 바람직하다.In addition, the extreme pressure additive as a sulfur-based additive, vegetable sulfide fat, mineral sulfide fat, mineral sulfide fat, lead thiamyl dithio carbamate, antimony dialkyl dithio carbamate, and antimony dialkyl phosphoro dithioate It is preferable to use 1 type or 2 types of mixtures chosen from.

이러한 극압첨가제는 극압하에서 높은 온도를 받아 분해되어 이황화몰리브덴(MoS2)이 형성되어 극압성을 높히고 마찰계수를 낮추는 효과를 나타낸다. 상기 극압첨가제의 사용함량은 0.5 ∼ 10 중량%로 사용하며, 이때 상기 극압첨가제의 함량이 상기 범위보다 과량이면 이황화몰리브덴의 분산력이 약화되고 침전되어 슬러지 합성이 일어나는 역작용이 나타나는 문제가 있으며, 반면에 상기범위를 초과하여 소량인 경우에는 고온고압하에서 분해되어 형성되는 이황화몰리브덴 화합물과 인화합물이 필요량보다 적어 요구되는 극압성 향상이 되지않고 마찰계수를 낮추는 효과가 없어지게 된다.These extreme pressure additives are decomposed under high temperature under extreme pressure to form molybdenum disulfide (MoS 2 ), thereby increasing the extreme pressure and lowering the friction coefficient. The use amount of the extreme pressure additive is 0.5 to 10% by weight, and if the content of the extreme pressure additive is more than the above range, there is a problem in that the dispersing force of molybdenum disulfide is weakened and precipitated, causing sludge synthesis to occur, whereas In the case of a small amount exceeding the above range, the molybdenum disulfide compound and the phosphorus compound formed by decomposition under high temperature and high pressure are less than the required amount, so that the required extreme pressure is not improved and the effect of lowering the friction coefficient is lost.

또한, 본 발명의 그리스 조성물은 전체 조성물 중의 유황 및 인 성분의 함량을 0.5 ∼ 3 중량%가 되도록 유지하는 것을 특징으로 하며, 이때 그 함량이 3 중량%를 초과하여 너무 과다하게 되면 극압성은 좋으나 금속에 대한 부식성이 커지기 때문에 바람직하지 않다.In addition, the grease composition of the present invention is characterized by maintaining the content of sulfur and phosphorus components in the total composition to be 0.5 to 3% by weight, when the content is too much exceeding 3% by weight, the extreme pressure is good but metal It is not preferable because the corrosiveness to is increased.

이상에서와 같이, 본 발명에서 내마모성의 효과는 유황과 완전히 공유 결합을 하고 있는 몰리브덴 복합체, 즉 유기몰리브덴 화합물이 극압을 받아 높은 온도에서 분해되어 이황화몰리브덴(MoS)이 형성되기 때문에 금속표면에 무기물층이 형성되어 표면융착 및 마모를 방지하게 되며, 이때 황화유지나 다른 극압제는 대부분 탄화수소기가 함유되어 있어 몰리브덴에 의한 촉매 작용으로 고분자물이 생성되어 윤활 금속면을 피복함으로써 마모 방지 효과를 상승시키고, 또한 인화물은 윤활면에서 마찰 계수를 낮추는 역할을 하는 것이다.As described above, the wear-resistant effect in the present invention is because the molybdenum complex, ie, the organic molybdenum compound, which is completely covalently bonded with sulfur, is decomposed at extreme temperatures to form molybdenum disulfide (MoS) to form an inorganic layer on the metal surface. This prevents surface fusion and abrasion. At this time, sulfide oils and other extreme pressure agents contain hydrocarbon groups, and thus, polymers are generated by the catalytic action of molybdenum to cover the lubricated metal surface, thereby increasing the wear protection effect. Phosphorus lowers the coefficient of friction in terms of lubrication.

이하, 본 발명을 실시예에 의하여 더욱 상세히 설명하면 다음과 같은 바, 본 발명이 이들 실시예에 의해 한정되는 것은 아니다.Hereinafter, the present invention will be described in more detail with reference to the following Examples, which are not intended to limit the present invention.

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

다음 표 1에 나타낸 바와 같은 함량 및 조성으로 통상의 방법을 이용하여 그리스 조성물을 제조하였다. 그리고, 다음의 각 방법으로 극압측정 및 사구 마모 측정을 하여 그 결과를 표 1에 요약하여 함께 나타내었다.The grease compositions were prepared using conventional methods in the amounts and compositions as shown in Table 1 below. In addition, extreme pressure measurement and glomerular wear measurement were performed by the following methods, and the results are summarized in Table 1 together.

(1) 쉘 4-볼(BALL) 극압시험: ASTM D 2596에 규정된 방법으로 시험하였다. 시험기 회전수 1,760 ±40 rpm, 시료온도 18 ∼ 35 ℃로 하고, 10초 간격으로 부하를 증가시켜 가면서 융착이 일어날 때까지 시험을 계속하였다.(1) Shell 4-Ball Extreme Pressure Test: Tested by the method specified in ASTM D 2596. The test was continued at 1,760 ± 40 rpm of the tester and at a sample temperature of 18 to 35 DEG C, while increasing the load at 10 second intervals until fusion occurred.

(2) 4-볼(BALL) 웨어(WEAR) 시험(사구마모테스트): ASTM D 2596에 규정된 방법으로 시험하였다.(2) 4-BALL WEAR test (sag wear test): Tested by the method specified in ASTM D 2596.

상기 표 1의 결과로 부터 알 수 있듯이, 같은 종류의 그리스를 사용했더라도 유기몰리브덴 성분과 극압제 성분을 각각 단독으로 사용하는 비교예보다 유기몰리브덴 성분과 극압제 성분을 동시에 혼합 사용하는 실시예의 경우가 마모수치나 마모량이 적게 일어났으며 부식도 적게 일어났으며, 내마모성도 비교예에 비해 더 양호하게 나타났다.As can be seen from the results of Table 1, even in the case of using the same type of grease, compared to the case of using the organic molybdenum component and the extreme pressure component simultaneously compared to the comparative example of using the organic molybdenum component and the extreme pressure component alone Abrasion value and abrasion occurred less, corrosion occurred less, and abrasion resistance was better than that of the comparative example.

이상에서 상세히 설명한 바와 같이, 본 발명에 따른 유기화합물 및 극압첨가제를 포함시켜 혼합 사용하는 그리스 조성물은 극압성과 내마모성이 최고 2배까지 향상되는 효과를 나타낸다.As described in detail above, the grease composition used in combination with the organic compound and the extreme pressure additive according to the present invention has an effect of improving the extreme pressure and wear resistance up to two times.

Claims (4)

기유, 유기화합물 및 극압첨가제로 이루어진 그리스 조성물에 있어서, 상기 그리스 조성물 중에 유기 몰리브덴 화합물 0.5 ∼ 10 중량% 및 극압첨가제 0.5 ∼ 10 중량%를 포함하되, 전체 그리스 조성물 중에 유황 및 인 성분의 함량이 0.5 ∼ 3 중량%인 것임을 특징으로 하는 극압 및 내마모성 그리스 조성물.A grease composition comprising a base oil, an organic compound, and an extreme pressure additive, comprising 0.5 to 10% by weight of an organic molybdenum compound and 0.5 to 10% by weight of an extreme pressure additive in the grease composition, wherein the sulfur and phosphorus content is 0.5 in the total grease composition. Extreme pressure and wear resistant grease composition, characterized in that from 3% by weight. 제 1 항에 있어서, 상기 유기 몰리브덴 화합물은 유황이 함유되지 않은 유기몰리브덴 화합물 또는 몰리브덴-유황 복합체인 것을 특징으로 하는 극압 및 내마모성 그리스 조성물.2. The extreme pressure and wear resistant grease composition according to claim 1, wherein the organic molybdenum compound is a sulfur-free organomolybdenum compound or a molybdenum-sulfur composite. 제 1 항 또는 제 2 항에 있어서, 상기 유기 몰리브덴 화합물이 다음 화학식 1로 표시되는 것임을 특징으로 하는 극압 및 내마모성 그리스 조성물:The extreme pressure and wear resistant grease composition according to claim 1 or 2, wherein the organic molybdenum compound is represented by the following Chemical Formula 1: 화학식 1Formula 1 상기 화학식 1에서, n은 1일 때 x는 1 ∼ 7의 정수이고, n은 2일 때 x는 1 ∼ 6의 정수이고, R은 하이드로카빌기, 알킬기, 아릴기, 알알킬기(aralkyl), 사이클로알킬기 또는 알카릴기(alkaryl)이다.In Formula 1, when n is 1, x is an integer of 1 to 7, when n is 2, x is an integer of 1 to 6, R is a hydrocarbyl group, an alkyl group, an aryl group, an alalkyl group, Cycloalkyl group or alkaryl group. 제 1 항에 있어서, 상기 극압첨가제는 식물성 황화유지, 광물성 황화유지, 납티아밀 디티오카바메이트, 안티몬 디알킬 디티오카바메이트, 및 안티몬 디알킬 포스포로 디티오에이트 중에서 선택되는 1 종 또는 2 종의 혼합물인 것임을 특징으로 하는 극압 및 내마모성 그리스 조성물.The method according to claim 1, wherein the extreme pressure additive is one or two selected from vegetable sulfide oil, mineral sulfide oil, lead thiamyl dithiocarbamate, antimony dialkyl dithiocarbamate, and antimony dialkyl phosphoro dithioate. Extreme pressure and wear resistant grease composition, characterized in that it is a mixture of species.
KR1020010023372A 2001-04-30 2001-04-30 Grease composite of extreme pressure and wear preventive characteristics KR20020083754A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100652123B1 (en) * 2005-12-13 2006-12-01 한국화학연구원 Vegetable modified mo-coordinative anti-wear additive with improved anti-wear property for greases and preparation method thereof
CN115992023A (en) * 2021-10-19 2023-04-21 中国石油化工股份有限公司 Lubricating grease and preparation method thereof
CN115992022A (en) * 2021-10-18 2023-04-21 中国石油化工股份有限公司 Lubricating grease and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100652123B1 (en) * 2005-12-13 2006-12-01 한국화학연구원 Vegetable modified mo-coordinative anti-wear additive with improved anti-wear property for greases and preparation method thereof
CN115992022A (en) * 2021-10-18 2023-04-21 中国石油化工股份有限公司 Lubricating grease and preparation method thereof
CN115992023A (en) * 2021-10-19 2023-04-21 中国石油化工股份有限公司 Lubricating grease and preparation method thereof

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